hexadecan-1-amine

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 66.4 g of hexadecylamine are dissolved in 250 ml of methanol. 27 ml of methyl acrylate are added and the mixture is left to stand overnight. After removal of the solvent by distillation the residue is recrystallised from ethyl acetate. the mixture is left After removal of the solvent by distillation the residue is recrystallised from ethyl acetate

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

実験手順: 30 g of hexadecylamine was dissolved in 250 liters of acetone. To this solution was added gradually a solution of 40 g of 1-acetoxy-5-acetaminonaphthalene-2-sulfonyl chloride synthesized above in 150 ml of acetone while stirring, and, after completion of the addition, stirring was continued for about 1 hour at about 40° C. Then, the reaction solution was cooled with ice, and the precipitated crystals were collected by filtration and well washed with 1 liter of methanol. The crystals were refluxed for 8 hours together with 200 ml of ethanol, 30 g of sodium hydroxide and 100 ml of water. After being allowed to cool to room temperature, the solution was neutralized with acetic acid, and the crystals thus precipitated were collected by filtration and recrystallized from an ethanol-water mixture solvent to obtain 22 g (54% yield) of product. after completion of the addition stirring Then, the reaction solution was cooled with ice the precipitated crystals were collected by filtration well washed with 1 liter of methanol The crystals were refluxed for 8 hours together with 200 ml of ethanol, 30 g of sodium hydroxide and 100 ml of water the crystals thus precipitated were collected by filtration recrystallized from an ethanol-water mixture solvent

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

実験手順: A 2 L two neck round bottom flask equipped with condenser was charged with D(+) glucose (60 g, 0.333 moles), 2-propanol (900 mL), hexadecylamine (81 g, 0.334 moles) and deionized water (300 mL). The reaction was stirred and heated to 50°-55° celsius for 1 hour to obtain a homogeneous solution. The reaction was then allowed to run overnight at room temperature. The reaction precipitated out after 2-3 hours. heated to 50°-55° celsius for 1 hour to obtain a homogeneous solution The reaction precipitated out after 2-3 hours

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

実験手順: Into a 1 l rounded-flask, were introduced 48.2 g of hexadecyl amine and 700 ml of ethanol. The mixture was heated to reflux, and then was gradually added 11 ml of 2-(2-chloroethoxy)ethanol. The mixture was refluxed for 3 hours and cooled to a room temperature. Thereto was added solution of KOH/ethanol to produce precipitates, which were removed by filtration. The filtrate was concentrated under reduced pressure, and then was recrystallized from ethanol, and dried to give 24.1 g of the title compound(Yield: 70%) as white powder, which was identified by IR and NMR. The results are shown in Table 1. The mixture was heated to reflux The mixture was refluxed for 3 hours to produce precipitates which were removed by filtration The filtrate was concentrated under reduced pressure was recrystallized from ethanol dried

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

実験手順: 800 g of 3-nitro 4-chlorobenzenesulfonylchloride and 1,000 ml of dichloromethane were mixed. A dichloromethane solution of 600 g of hexadecylamine and 251 ml of triethylamine was added dropwise to the mixture. After the reaction was finished, the reaction solvent was removed under reduced pressure. 3,000 ml of methanol was added to the system. The mixture was then heated so that dissolution was effected. The solution was then gradually cooled. As a result, crystals precipitated. The crystals were then filtered off, and dried. the reaction solvent was removed under reduced pressure 3,000 ml of methanol was added to the system The mixture was then heated so that dissolution The solution was then gradually cooled As a result, crystals precipitated The crystals were then filtered off dried

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

実験手順: 800 g of 3-nitro 4-chlorobenzenesulfonylchloride and 1,000 ml of dichloromethane were mixed. A dichloromethane solution of 600 g of hexadecylamine and 251 ml of triethylamine was added dropwise to the mixture. After the reaction was finished, the reaction solvent was removed under reduced pressure. 3,000 ml of methanol was added to the system. The mixture was then heated so that dissolution was effected. The solution was then gradually cooled. As a result, crystals precipitated. The crystals were then filtered off, and dried. the reaction solvent was removed under reduced pressure 3,000 ml of methanol was added to the system The mixture was then heated so that dissolution The solution was then gradually cooled As a result, crystals precipitated The crystals were then filtered off dried

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

実験手順: A mixture of 59.45 g of hexadecylamine, 10.60 g of gamma butyrolactone, 200 ml of toluene, and 20 mg of zinc chloride was refluxed under nitrogen for three days. Upon cooling, the reaction mixture formed a precipitate which was recrystallized twice from toluene to yield 31.5 g (78.12%) of N-hexadecyl-4-hydroxybutyramide, m.p. 89.5°-90° was refluxed under nitrogen for three days Upon cooling the reaction mixture formed a precipitate which was recrystallized twice from toluene

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 0.5 g (3.2 mmol) of 2-chloro-5-nitropyridine (Fluka, purum), 0.76 g (3.2 mmol) of hexadecylamine (Merck-Schuchard, for synthesis) and 1 g of NaHCO3 are weighed out and suspended in 10 ml of CHCl3 /DMF 1:1 (puriss., for analysis). The suspension is heated to 100° C. (bath temperature) and stirred for 4 hours at this temperature. When the reaction mixture has cooled, water is added and extraction is carried out with diethyl ether. The organic phase is extracted twice with water and dried over Na2SO4. After evaporation of the solvent, the residue is chromatographed on 50 times the amount of silica gel (eluent=hexane/ether 95:5). The slightly yellowish product fraction is concentrated and 1 is recrystallized again from hexane/ether. When the reaction mixture has cooled extraction The organic phase is extracted twice with water dried over Na2SO4 After evaporation of the solvent the residue is chromatographed on 50 times the amount of silica gel (eluent=hexane/ether 95:5) The slightly yellowish product fraction is concentrated 1 is recrystallized again from hexane/ether

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 0.5 g (3.2 mmol) of 2-chloro-5-nitropyridine (Fluka, purum), 0.76 g (3.2 mmol) of hexadecylamine (Merck-Schuchard, for synthesis) and 1 g of NaHCO3 are weighed out and suspended in 10 ml of CHCl3 /DMF 1:1 (puriss., for analysis). The suspension is heated to 100° C. (bath temperature) and stirred for 4 hours at this temperature. When the reaction mixture has cooled, water is added and extraction is carried out with diethyl ether. The organic phase is extracted twice with water and dried over Na2SO4. After evaporation of the solvent, the residue is chromatographed on 50 times the amount of silica gel (eluent=hexane/ether 95:5). The slightly yellowish product fraction is concentrated and 1 is recrystallized again from hexane/ether. When the reaction mixture has cooled extraction The organic phase is extracted twice with water dried over Na2SO4 After evaporation of the solvent the residue is chromatographed on 50 times the amount of silica gel (eluent=hexane/ether 95:5) The slightly yellowish product fraction is concentrated 1 is recrystallized again from hexane/ether