calcium;diacetate;hydrate

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

実験手順: N-ethyl-N-phenyl-5-ethyl-1,2-dihydro-4-hydroxy-1-methyl-2-oxo-3-quinolinecarboxamide (28.5 mmol, 10.0 g) was dissolved in a mixture of water (200 mL) and 10M NaOH (28.5 mmol, 2.85 mL), and pH was adjusted to 7.5-8.0 with 1M HCl. To this solution at 50° C. was added during 15 min a solution of calcium acetate hydrate (15 mmol, 2.67 g) in water (50 ml) and the resultant thick emulsion was allowed to cool to room temperature and the precipitate was filtered and washed with water. The precipitate was dried in vacuum to give 8.96 g of an amorphous calcium salt. the precipitate was filtered washed with water The precipitate was dried in vacuum

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Ethyl-N-phenyl-5-chloro-1,2-dihydro-4-hydroxy-1-methyl-2-oxo-3-quinolinecarboxamide sodium salt (2.63 mmol, 1.0 g) was dissolved in a mixture of ethanol (10.5 ml) and water (5.3 ml). The solution was heated to 70° C. and a solution of calcium acetate hydrate in water (1M solution, 1.05 eq., 1.38 mmol, 1.38 ml) was added. The resulting suspension was stirred for 30 minutes, then cooled, and the crystals were isolated by filtration, washed with water, and dried under vacuum (966 mg, 98% yield). Anal. Calcd for C38H32Cl2N4O6Ca: C, 60.7; H, 4.29; N, 7.45. Found C, 60.5; H, 4.34; N, 7.41. cooled the crystals were isolated by filtration washed with water dried under vacuum (966 mg, 98% yield)

反応条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Mixture of 100 g (0.186 mol) (3S)-tetrahydro-3-furyl N-[(1S,2R)-1-benzyl-2-hydroxy-3-(N-isobutyl-4-nitrobenzene sulphonamido)propyl]carbamate (IV) and 200 ml pyridine was cooled to 0-10° C. and 70.0 g (0.456 mol) of POCl3 was added and stirred at ambient temperature for 4 hours, 400 ml methyl isobutyl ketone was added, cooled and 1:1 conc. HCl-water was added. Mixture was heated to 50° C. for 1 hour, cooled to 25-30° C. Organic layer was separated, washed with water and partially concentrated; 500 ml water and 31.5 g sodium bicarbonate was added and stirred. The organic layer was separated and 100 ml ethylacetate, 400 ml methanol and 5.0 g Pd/C was added. The reaction mass was stirred under hydrogen pressure for 4 hours at 30° C. The mixture was filtered, catalyst washed with methanol. The filtrate was heated to 50° C. and 33.0 g (0.186 mol) calcium acetate monohydrate in 100 ml water was added and stirred for 30 minutes. Cooled to 30° C. and stirred. Solid was filtered, washed with 1:1 mixture of methanol-water and dried to obtain crude fosamprenavir calcium. cooled Mixture was heated to 50° C. for 1 hour cooled to 25-30° C Organic layer was separated washed with water partially concentrated 500 ml water and 31.5 g sodium bicarbonate was added stirred The organic layer was separated 100 ml ethylacetate, 400 ml methanol and 5.0 g Pd/C was added The reaction mass was stirred under hydrogen pressure for 4 hours at 30° C The mixture was filtered catalyst washed with methanol The filtrate was heated to 50° C. stirred for 30 minutes Cooled to 30° C. stirred Solid was filtered washed with 1:1 mixture of methanol-water dried

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

実験手順: An aqueous solution of 8.51 g 50 wt % H3PO2 was combined with 8.00 g of 25.0 wt % aqueous solution of calcium acetate monohydrate, Ca(O2CCH3)2.H2O (ACS reagent, Aldrich Chemical Co., Inc. #40,285-0, CAS 5743-26-0), equivalent to 5.69 wt % Ca, to give a clear, colorless solution contained in a 250 ml Pyrex beaker. To this solution was added 20.17 g Ca(NO3)2.4H2O salt. The molar ratio of Ca/phosphate in this mixture was 3/2 and the equivalent solids level [as Ca3(PO4)2] was 27.3 wt %. Endothermic dissolution of the calcium nitrate tetrahydrate salt proceeded giving a homogeneous solution once the sample warmed to room temperature. Further warming of this solution to >25° C. on a hotplate initiated a reaction which proceeded as described in Example 1. After approximately three minutes, the reaction was essentially complete leaving a moist, white, crumbly solid which was hot to the touch and which smelled of acetic acid. After cooling to room temperature, the solid was stored in a polyethylene vial. proceeded giving a homogeneous solution once the sample Further warming of this solution to >25° C. on a hotplate a reaction which the reaction was essentially complete leaving a moist, white, crumbly solid which After cooling to room temperature

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

実験手順: An aqueous solution of 8.51 g 50 wt % H3PO2 was combined with 8.00 g of 25.0 wt % aqueous solution of calcium acetate monohydrate, Ca(O2CCH3)2.H2O (ACS reagent, Aldrich Chemical Co., Inc. #40,285-0, CAS 5743-26-0), equivalent to 5.69 wt % Ca, to give a clear, colorless solution contained in a 250 ml Pyrex beaker. To this solution was added 20.17 g Ca(NO3)24.H2O salt. The molar ratio of Ca/phosphate in this mixture was 3/2 and the equivalent solids level [as Ca3(PO4)2] was 27.3 wt %. Endothermic dissolution of the calcium nitrate tetrahydrate salt proceeded giving a homogeneous solution once the sample warmed to room temperature. Further warming of this solution to >25° C. on a hotplate initiated a reaction which proceeded as described in Example 1. After approximately three minutes, the reaction was essentially complete leaving a moist, white, crumbly solid which was hot to the touch and which smelled of acetic acid. After cooling to room temperature, the solid was stored in a polyethylene vial. proceeded giving a homogeneous solution once the sample Further warming of this solution to >25° C. on a hotplate a reaction which the reaction was essentially complete leaving a moist, white, crumbly solid which After cooling to room temperature

反応条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1.4 moles of dimethyl terephthalate (277 g) and 7.2 moles of ethylene glycol (445 g) were weighed into a one-liter round-bottomed flask connected to a vacuum line. A catalytic amount of cobalt (II) acetate tetrahydrate (180 mg, 0.5 mole) and calcium acetate hydrate (90 mg, 0.4 mole) were added. The reaction mixture was heated at 160° C. in an oil bath under a mild vacuum.

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

実験手順: An aqueous solution of 8.51 g 50 wt % H3PO2 was combined with 8.00 g of 25.0 wt % aqueous solution of calcium acetate monohydrate, Ca(O2CCH3)2.H2O (ACS reagent, Aldrich Chemical Co., Inc. #40,285-0, CAS 5743-26-0), equivalent to 5.69 wt % Ca, to give a clear, colorless solution contained in a 250 ml Pyrex beaker. To this solution was added 20.17 g Ca(NO3)2.4H2O salt. The molar ratio of Ca/phosphate in this mixture was 3/2 and the equivalent solids level [as Ca3(PO4)2] was 27.3 wt %. Endothermic dissolution of the calcium nitrate tetrahydrate salt proceeded giving a homogeneous solution once the sample warmed to room temperature. Further warming of this solution to >25° C. on a hotplate initiated a reaction which proceeded as described in Example 1. After approximately three minutes, the reaction was essentially complete leaving a moist, white, crumbly solid which was hot to the touch and which smelled of acetic acid. After cooling to room temperature, the solid was stored in a polyethylene vial. proceeded giving a homogeneous solution once the sample Further warming of this solution to >25° C. on a hotplate a reaction which the reaction was essentially complete leaving a moist, white, crumbly solid which After cooling to room temperature

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

実験手順: An aqueous solution of 8.51 g 50 wt % H3PO2 was combined with 8.00 g of 25.0 wt % aqueous solution of calcium acetate monohydrate, Ca(O2CCH3)2.H2O (ACS reagent, Aldrich Chemical Co., Inc. #40,285-0, CAS 5743-26-0), equivalent to 5.69 wt % Ca, to give a clear, colorless solution contained in a 250 ml Pyrex beaker. To this solution was added 20.17 g Ca(NO3)24H2O salt. The molar ratio of Ca/phosphate in this mixture was 3/2 and the equivalent solids level [as Ca3(PO4)2] was 27.3 wt %. Endothermic dissolution of the calcium nitrate tetrahydrate salt proceeded giving a homogeneous solution once the sample warmed to room temperature. Further warming of this solution to >25° C. on a hotplate initiated a reaction which proceeded as described in Example 1. After approximately three minutes, the reaction was essentially complete leaving a moist, white, crumbly solid which was hot to the touch and which smelled of acetic acid. After cooling to room temperature, the solid was stored in a polyethylene vial. proceeded giving a homogeneous solution once the sample Further warming of this solution to >25° C. on a hotplate a reaction which the reaction was essentially complete leaving a moist, white, crumbly solid which After cooling to room temperature

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

実験手順: The preparation of the immobilized enzyme and the reaction were conducted in the same manner as in Example 1 with the exception that: The quantity of Thermoase and that of the calcium acetate monohydrate were 9.0 g and 0.45 g respectively, the quantity of the 0.05 M sodium acetate buffer solution of pH 7.5 was 90 ml; the acrylic ester matrix carrier (Amberlite XAD-7, Trademark) was replaced with 16.6 g of another carrier of the similar class (Amberlite XAD-8, Trademark, containing about 150 wt.% of water on a dry basis; the quantity of N-benzyloxycarbonyl-L-aspartic acid was 2.14 g (8 m mol): L-phenylalanine methyl ester was replaced with 2.87 g (16 m mol) of DL-phenylalanine methyl ester; the quantity of the water saturated ethyl acetate solution was changed to 26 ml; and the reaction time was five fours. N-Benzyloxycarbonyl-L-aspartyl-L-phenylalanine methyl ester was obtained in the yield of 79.8%. The preparation of the immobilized enzyme

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Ethyl-N-phenyl- 5-ethyl- 1,2-dihydro- 4-hydroxy- 1-methyl- 2-oxo- 3-quinolinecarboxamide ( 5.0 g, 14.2 mmol) was dissolved in a mixture of 1M NaOH ( 14.26 mmol, 14.26 ml) and ethanol ( 30 ml), and pH was adjusted to 7.5. The solution was heated to 70° C. and calcium acetate hydrate ( 1.05 eq., 7.5 mmol, 1.335 g) in water ( 7 ml) was added dropwise during 5 min. The heating was discontinued and the mixture was stirred at room temperature for 1 h, the crystals were filtered, washed with ethanol/water 1/l and dried under vacuum to afford the title compound ( 5.16 g, 98% yield). Anal. Calcd for C42H42N4O6Ca: C, 68.3; H, 5.73; N, 7.58. Found C, 68.4; H, 5.72; N, 7.63. EDTA-titriometric determination of calcium gave a content of 5.42% (theoretical content is 5.42%). the crystals were filtered washed with ethanol/water 1/l dried under vacuum

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Ethyl-N-phenyl- 5-ethyl- 1,2-dihydro- 4-hydroxy- 1-methyl- 2-oxo- 3-quinolinecarboxamide ( 5.0 g, 14.2 mmol) was dissolved in a mixture of 1M NaOH ( 14.26 mmol, 14.26 ml) and ethanol ( 30 ml), and pH was adjusted to 7.5. The solution was heated to 70° C. and calcium acetate hydrate ( 1.05 eq., 7.5 mmol, 1.335 g) in water ( 7 ml) was added dropwise during 5 min. The heating was discontinued and the mixture was stirred at room temperature for 1 h, the crystals were filtered, washed with ethanol/water 1/l and dried under vacuum to afford the title compound ( 5.16 g, 98% yield). Anal. Calcd for C42H42N4O6Ca: C, 68.3; H, 5.73; N, 7.58. Found C, 68.4; H, 5.72; N, 7.63. EDTA-titriometric determination of calcium gave a content of 5.42% (theoretical content is 5.42%). the crystals were filtered washed with ethanol/water 1/l dried under vacuum

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Ethyl-N-phenyl- 5chloro- 1,2-dihydro- 4-hydroxy- 1-methyl- 2-oxo- 3-quinolinecarboxamide sodium salt ( 2.63 mmol, 1.0 g) was dissolved in a mixture of ethanol ( 10.5 ml) and water ( 5.3 ml). The solution was heated to 70° C. and a solution of calcium acetate hydrate in water ( 1M solution, 1.05 eq., 1.38 mmol, 1.38 ml) was added. The resulting suspension was stirred for 30 minutes, then cooled, and the crystals were isolated by filtration, washed with water, and dried under vacuum ( 966 mg, 98% yield). Anal. Calcd for C38H32Cl2N4O6Ca: C, 60.7; H, 4.29; N, 7.45. Found C, 60.5; H, 4.34; N, 7.41. cooled the crystals were isolated by filtration washed with water dried under vacuum ( 966 mg, 98% yield)