2-hydroxy-2-methylpropanamide

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Next, when 100 cc of an aqueous solution containing 20.3 g (0.143 mole) of sodium hydrogenphosphate (Na2HPO4) was added, a white precipitate was formed. After stirring this at 80° C. for one hour, the white precipitate was thoroughly water-washed by the decantation method followed by separation by filtration and water-washing. The resulting white precipitate was dried at 120° C., calcined at 400° C. for 6 hours in a stream of air, and thereafter molded into granules of 10-16-mesh size. The LaPO4 catalyst (5 cc) thus obtained was packed in a Pyrex reaction tube of 12-mm inside diameter, which then was secured in an electric furnace held at 275° C. Next, while passing nitrogen from the top of the reaction tube through the catalyst layer at a gas space velocity of 480 liter/liter/hr, 14% ammonia water was passed through the catalyst layer at a liquid hourly space velocity of 0.5 liter/liter/hr for 30 minutes. The feed of the ammonia water was then stopped, and a feed liquid consisting of α-hydroxyisobutyramide, methanol and water in a mole ratio of 1:14:11.5 was fed at a liquid hourly space velocity of 0.26 liter/liter/hr. The gas leaving the catalyst layer was trapped in a dry ice trap coupled to the bottom of the reaction tube. When the products were quantitatively analyzed by gas chromatography, the molar yields of methyl methacrylate and methacrylic acid were 83.2% and 3.0%, respectively, based on the starting α-hydroxyisobutyramide. was added a white precipitate was formed washed by the decantation method followed by separation by filtration and water- washing The resulting white precipitate was dried at 120° C. calcined at 400° C. for 6 hours in a stream of air The LaPO4 catalyst (5 cc) thus obtained was packed in a Pyrex reaction tube of 12-mm inside diameter, which held at 275° C was passed through the catalyst layer at a liquid hourly space velocity of 0.5 liter/liter/hr for 30 minutes The gas leaving the catalyst layer was trapped in a dry ice trap

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This preparation generally comprises the reaction of acetone cyanohydrin with concentrated sulphuric acid to give α-hydroxyisobutyramide and α-hydroxyisobutyramide sulphate. These two compounds are then heated to give sulphuric methacrylamide. This preparation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 20.6 g of α-hydroxy-isobutyramide and 204 g of n-hexyl alcohol was heated in the presence of 0.45 g of PbO for 6 hours at 200° C. in an autoclave. On working up by distillation, 19.5 g (= 51.8 percent of theory) of α-hydroxy-isobutyric acid-n-hexyl-ester were obtained. The amide conversion is 75 percent. On working up by distillation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: By way of example and not limitation, a description of the present invention, specifically the embodiment illustrated by FIG. 2, when used in an MMA process is provided. The most common feedstock for the production of MMA is acetone cyanohydrin (“ACH”). The first stage of producing MMA from ACH involves hydrolysis where the ACH is hydrolyzed by an excess of sulfuric acid to form alpha-sulfatoisobutyramide (“SIBAM”), alpha-hydroxyisobutyramide (“HIBAM”), methacrylamide (“MAM”), and MAA. Following hydrolysis, the hydrolysis mix is cracked to form MAM and a small amount of MAA, HIBAM and SIBAM. The cracked mix is then esterified with methanol to form valuable product MMA, but a sulfur-bearing residue stream is also produced that contains water, sulfuric acid, ammonium bisulfate, methanol, MMA, MAA, methanesulfonic acid and other trace components. It is desirable to recover the valuable organics from this residue stream and to concentrate the residue so that there is less residue to handle in downstream processing or disposal operations. To accomplish these goals, this sulfur-bearing upper flash tank feedstream is fed, for example, through conduit 22 into upper flash tank 24 where some of the water and organic components including MMA, MAA, and methanol are removed from the stream and taken overhead through conduit 21 to condenser 26. The remainder of the residue, which is primarily ammonium sulfate, ammonium bisulfate, sulfuric acid, water, acetone, disulfonic acid, methanol, MAA and MMA, exits flash tank 24 and is conveyed into stripping vessel 30 via conduit 28. In stripping vessel 30, separation occurs and valuable organics components like methanol, MMA and MAA along with water are taken overhead via conduit 23 to condenser 32. From condenser 32 and condenser 26, the recovered organics and water can be recycled back into the process or stored via conduit 27 and conduit 25, respectively. From stripping vessel 30, the stripping vessel residue stream, which is primarily ammonium sulfate, ammonium bisulfate, sulfuric acid, water, acetone disulfonic acid, methanol, MAA and MMA, is fed into lower flash tank 34 by conduit 36. While the stripping vessel residue stream is residing in lower flash tank 34, methanol is added to the residue via conduit 42 to induce chemical reactions between and among components of the stripping vessel residue stream to produce lighter organic components, specifically MMA from MAA and methanol. These organic components are recovered at condenser 32 via conduit 35, stripping vessel 30 and conduit 23. The lower flash tank residue stream exits lower flash tank 34 and is fed to heat exchanger 38 via conduits 31 and 33 and then refed into lower flash tank 34 via conduit 29 after exiting the heat exchanger. Once the optimal amount of organics have been recovered, the lower flash tank residue stream, which is primarily composed of ammonium sulfate, ammonium bisulfate, sulfuric acid, water, and acetone disulfonic acid, exits the residue treatment system at conduit 40 for further processing or disposal. is provided

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Next, when 100 cc of an aqueous solution containing 20.3 g (0.143 mole) of sodium hydrogenphosphate (Na2HPO4) was added, a white precipitate was formed. After stirring this at 80° C. for one hour, the white precipitate was thoroughly water-washed by the decantation method followed by separation by filtration and water-washing. The resulting white precipitate was dried at 120° C., calcined at 400° C. for 6 hours in a stream of air, and thereafter molded into granules of 10-16-mesh size. The LaPO4 catalyst (5 cc) thus obtained was packed in a Pyrex reaction tube of 12-mm inside diameter, which then was secured in an electric furnace held at 275° C. Next, while passing nitrogen from the top of the reaction tube through the catalyst layer at a gas space velocity of 480 liter/liter/hr, 14% ammonia water was passed through the catalyst layer at a liquid hourly space velocity of 0.5 liter/liter/hr for 30 minutes. The feed of the ammonia water was then stopped, and a feed liquid consisting of α-hydroxyisobutyramide, methanol and water in a mole ratio of 1:14:11.5 was fed at a liquid hourly space velocity of 0.26 liter/liter/hr. The gas leaving the catalyst layer was trapped in a dry ice trap coupled to the bottom of the reaction tube. When the products were quantitatively analyzed by gas chromatography, the molar yields of methyl methacrylate and methacrylic acid were 83.2% and 3.0%, respectively, based on the starting α-hydroxyisobutyramide. was added a white precipitate was formed washed by the decantation method followed by separation by filtration and water- washing The resulting white precipitate was dried at 120° C. calcined at 400° C. for 6 hours in a stream of air The LaPO4 catalyst (5 cc) thus obtained was packed in a Pyrex reaction tube of 12-mm inside diameter, which held at 275° C was passed through the catalyst layer at a liquid hourly space velocity of 0.5 liter/liter/hr for 30 minutes The gas leaving the catalyst layer was trapped in a dry ice trap

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This preparation generally comprises the reaction of acetone cyanohydrin with concentrated sulphuric acid to give α-hydroxyisobutyramide and α-hydroxyisobutyramide sulphate. These two compounds are then heated to give sulphuric methacrylamide. This preparation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This preparation generally comprises the reaction of acetone cyanohydrin with concentrated sulphuric acid to give α-hydroxyisobutyramide and α-hydroxyisobutyramide sulphate. These two compounds are then heated to give sulphuric methacrylamide. This preparation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: It is publicly known that manganese dioxide is used as a solid catalyst in the hydration reaction of acetone cyanohydrin. According to any of the conventional processes, α-hydroxyisobutyramide is obtained by the reaction of acetone cyanohydrin with water as shown by the following reaction equation at a temperature of 40° to 100° C. in the presence of manganese-based catalyst and preferably an acetone-based solvent in a yield of 60 to 95%.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: It is publicly known that manganese dioxide is used as a solid catalyst in the hydration reaction of acetone cyanohydrin. According to any of the conventional processes, α-hydroxyisobutyramide is obtained by the reaction of acetone cyanohydrin with water as shown by the following reaction equation at a temperature of 40° to 100° C. in the presence of manganese-based catalyst and preferably an acetone-based solvent in a yield of 60 to 95%.

反応条件: temp:240.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of commercially available 2-hydroxyisobutyramide (638.5 mg, 3 eq), 2-benzyloxy-6-methoxy-benzaldehyde (500 mg) (Katritzky A. R. et al ARKIVOC 2001, 2, 3, 3-12) is heated at 240° C. for 5 min using microwave irradiation (Lecolier S. et al Chimica Therapeutica 1969, 4,6, 437-445). The crude oil is poured into water and extracted with DCM. The combined organic extracts are dried (MgSO4), filtered and concentrated to yield a crude oil. FC (EN n-heptane: 1/1 to 1/0) gives the title compound as a yellow solid (0.41 g, 61%); LC-MS: tR=0.65 min; [M+H]+=328.22. microwave irradiation (Lecolier S. et al Chimica Therapeutica 1969, 4,6, 437-445) extracted with DCM The combined organic extracts are dried (MgSO4) filtered concentrated to yield a crude oil

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: By way of example and not limitation, a description of the present invention, specifically the embodiment illustrated by FIG. 2, when used in an MMA process is provided. The most common feedstock for the production of MMA is acetone cyanohydrin (“ACH”). The first stage of producing MMA from ACH involves hydrolysis where the ACH is hydrolyzed by an excess of sulfuric acid to form alpha-sulfatoisobutyramide (“SIBAM”), alpha-hydroxyisobutyramide (“HIBAM”), methacrylamide (“MAM”), and MAA. Following hydrolysis, the hydrolysis mix is cracked to form MAM and a small amount of MAA, HIBAM and SIBAM. The cracked mix is then esterified with methanol to form valuable product MMA, but a sulfur-bearing residue stream is also produced that contains water, sulfuric acid, ammonium bisulfate, methanol, MMA, MAA, methanesulfonic acid and other trace components. It is desirable to recover the valuable organics from this residue stream and to concentrate the residue so that there is less residue to handle in downstream processing or disposal operations. To accomplish these goals, this sulfur-bearing upper flash tank feedstream is fed, for example, through conduit 22 into upper flash tank 24 where some of the water and organic components including MMA, MAA, and methanol are removed from the stream and taken overhead through conduit 21 to condenser 26. The remainder of the residue, which is primarily ammonium sulfate, ammonium bisulfate, sulfuric acid, water, acetone, disulfonic acid, methanol, MAA and MMA, exits flash tank 24 and is conveyed into stripping vessel 30 via conduit 28. In stripping vessel 30, separation occurs and valuable organics components like methanol, MMA and MAA along with water are taken overhead via conduit 23 to condenser 32. From condenser 32 and condenser 26, the recovered organics and water can be recycled back into the process or stored via conduit 27 and conduit 25, respectively. From stripping vessel 30, the stripping vessel residue stream, which is primarily ammonium sulfate, ammonium bisulfate, sulfuric acid, water, acetone disulfonic acid, methanol, MAA and MMA, is fed into lower flash tank 34 by conduit 36. While the stripping vessel residue stream is residing in lower flash tank 34, methanol is added to the residue via conduit 42 to induce chemical reactions between and among components of the stripping vessel residue stream to produce lighter organic components, specifically MMA from MAA and methanol. These organic components are recovered at condenser 32 via conduit 35, stripping vessel 30 and conduit 23. The lower flash tank residue stream exits lower flash tank 34 and is fed to heat exchanger 38 via conduits 31 and 33 and then refed into lower flash tank 34 via conduit 29 after exiting the heat exchanger. Once the optimal amount of organics have been recovered, the lower flash tank residue stream, which is primarily composed of ammonium sulfate, ammonium bisulfate, sulfuric acid, water, and acetone disulfonic acid, exits the residue treatment system at conduit 40 for further processing or disposal. is provided

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: At the step (III) of Example 1, the reaction was carried out in the same manner as in Example 1 except that an aqueous solution was used in place of the N-methylpyrrolidone solution. As a result, the conversion of the α-hydroxyisobutyric acid amide as starting material was 98.6%, and the yield of methacrylic acid amide based on the converted starting material was 41.8 ol %. In addition, 32% of methacrylic acid, 10% of acetone, and 8% of methacrylonitrile were formed.