N-(Tetrahydro-2-oxo-3-thienyl)-acetamide

Conditions: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To the solution of phosphoryl chloride 14.9 ml (160 mmol) in dimethylformamide 45 ml, N-(2-oxotetrahydrothiophen-3-yl)acetamide 12.74 g (80 mmol) was added portion wise and stirred at 90° C. for 2 hours. The reaction mixture was poured into ice water 400 ml and followed by addition of saturated sodium acetate 500 ml. The solution was extracted by ethyl acetate 1000 ml. The organic phase was washed with water 300 ml and brine 200 ml. Then the organic phase was dried over magnesium sulfate, filtered and concentrated. The residue was crystallized by addition of ethyl acetate/ether (1:1) 200 ml and filtered. The filtrate was concentrated to obtain the title compound 3.55 g (18%). The solution was extracted by ethyl acetate 1000 ml The organic phase was washed with water 300 ml and brine 200 ml Then the organic phase was dried over magnesium sulfate filtered concentrated The residue was crystallized by addition of ethyl acetate/ether (1:1) 200 ml filtered The filtrate was concentrated

Conditions: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To the solution of phosphoryl chloride 14.9 ml (160 mmol) in dimethylformamide 45 ml, N-(2-oxotetrahydrothiophen-3-yl)acetamide 12.74 g (80 mmol) was added portion wise and stirred at 90° C. for 2 hours. The reaction mixture was poured into ice water 400 ml and followed by addition of saturated sodium acetate 500 ml. The solution was extracted by ethyl acetate 1000 ml. The organic phase was washed with water 300 ml and brine 200 ml. Then the organic phase was dried over magnesium sulfate, filtered and concentrated. The residue was crystallized by addition of ethyl acetate/ether (1:1) 200 ml and filtered. The filtrate was concentrated to obtain the title compound 3.55 g (18%). The solution was extracted by ethyl acetate 1000 ml The organic phase was washed with water 300 ml and brine 200 ml Then the organic phase was dried over magnesium sulfate filtered concentrated The residue was crystallized by addition of ethyl acetate/ether (1:1) 200 ml filtered The filtrate was concentrated

Conditions: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a solution of phosphoryl chloride (14.9 ml, 160 mmol) in dimethylformamide (45 ml) was added portionwise N-(2-oxotetrahydrothiophen-3-yl)acetamide (12.74 g, 80 mmol) and the mixture was stirred at 90° C. for 2 hr. The reaction mixture was poured into ice water (400 ml) and followed by addition of saturated sodium acetate (500 ml). The solution was extracted by ethyl acetate (1000 ml). The organic layer was washed with water (300 ml), water (400 ml) and brine (200 ml). Then the organic layer was dried over magnesium sulfate, filtered and the filtrate was concentrated in vacuo. The residue was crystallized by addition of ethyl acetate/ether (1:1, 200 ml) and the crystals were collected by filtration to obtain the title compound (3.55 g, 18%). The solution was extracted by ethyl acetate (1000 ml) The organic layer was washed with water (300 ml), water (400 ml) and brine (200 ml) Then the organic layer was dried over magnesium sulfate filtered the filtrate was concentrated in vacuo The residue was crystallized by addition of ethyl acetate/ether (1:1, 200 ml) the crystals were collected by filtration

Conditions: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a solution of phosphoryl chloride (14.9 ml, 160 mmol) in dimethylformamide (45 ml) was added portionwise N-(2-oxotetrahydrothiophen-3-yl)acetamide (12.74 g, 80 mmol) and the mixture was stirred at 90° C. for 2 hr. The reaction mixture was poured into ice water (400 ml) and followed by addition of saturated sodium acetate (500 ml). The solution was extracted by ethyl acetate (1000 ml). The organic layer was washed with water (300 ml), water (400 ml) and brine (200 ml). Then the organic layer was dried over magnesium sulfate, filtered and the filtrate was concentrated in vacuo. The residue was crystallized by addition of ethyl acetate/ether (1:1, 200 ml) and the crystals were collected by filtration to obtain the title compound (3.55 g, 18%). The solution was extracted by ethyl acetate (1000 ml) The organic layer was washed with water (300 ml), water (400 ml) and brine (200 ml) Then the organic layer was dried over magnesium sulfate filtered the filtrate was concentrated in vacuo The residue was crystallized by addition of ethyl acetate/ether (1:1, 200 ml) the crystals were collected by filtration

Conditions: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: NaOH (1 M deoxygenated aqueous solution, 100 mL) was dropwise added to DL-N-acetylhomocysteine thiolactone (4.00 g, 25.124 mmol). Addition time: 15 min. The reaction mixture was warmed up to 50° C. and allowed to react for 30 min. The reaction was cooled down to 0° C., acidified with HCl (10% aqueous solution, 30 mL) and the product was extracted with nBuOH (4×70 mL). The organic layer was dried over Na2SO4 (anhydrous), filtered and concentrated. The crude residue was slurred with Et2O/hexanes (1:3, 150 mL) to furnish 4.00 g of DL-N-acetylhomocysteine (white solid, yield: 90%). Addition time 15 min to react for 30 min The reaction was cooled down to 0° C. the product was extracted with nBuOH (4×70 mL) The organic layer was dried over Na2SO4 (anhydrous) filtered concentrated

Conditions: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To the solution of phosphoryl chloride 14.9 ml (160 mmol) in dimethylformamide 45 ml, N-(2-oxotetrahydrothiophen-3-yl)acetamide 12.74 g (80 mmol) was added portion wise and stirred at 90° C. for 2 hours. The reaction mixture was poured into ice water 400 ml and followed by addition of saturated sodium acetate 500 ml. The solution was extracted by ethyl acetate 1000 ml. The organic phase was washed with water 300 ml and brine 200 ml. Then the organic phase was dried over magnesium sulfate, filtered and concentrated. The residue was crystallized by addition of ethyl acetate/ether (1:1) 200 ml and filtered. The filtrate was concentrated to obtain the title compound 3.55 g (18%). The solution was extracted by ethyl acetate 1000 ml The organic phase was washed with water 300 ml and brine 200 ml Then the organic phase was dried over magnesium sulfate filtered concentrated The residue was crystallized by addition of ethyl acetate/ether (1:1) 200 ml filtered The filtrate was concentrated