2-甲基亚磺酰基乙酰胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a cold (-70° C.) solution of 12.77 g (0.055 mole) of 2-amino-5-chlorobenzophenone in 300 mL of methylene chloride, under nitrogen atmosphere, was added 6.0 g (0.552 mole) of t-butylhypochlorite in 20 mL of methylene chloride. After the reaction was stirred for an additional 15 min, a suspension of 5.8 g (0.055 mole) of α-(methylthio)acetamide in 150 mL of methylene chloride was added. The mixture was stirred at -65° C. for 1 h. Triethylamine (5.6 g, 0.055 mole) was added and the solution was allowed to warm to room temperature. The reaction mixture was extracted with water and the organic layer dried over magnesium sulfate. The volume of the solution was reduced in vacuo to about 200 mL and the product crystallized as a yellow solid, m.p. 173.5°-174.5° C. Yield was 6.86 g (37.3%). was added The mixture was stirred at -65° C. for 1 h The reaction mixture was extracted with water the organic layer dried over magnesium sulfate the product crystallized as a yellow solid, m.p. 173.5°-174.5° C

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a cold (-70° C.) solution of 12.77 g (0.055 mole) of 2-amino-5-chlorobenzophenone in 300 mL of methylene chloride, under nitrogen atmosphere, was added 6.0 g (0.552 mole) of t-butylhypochlorite in 20 mL of methylene chloride. After the reaction was stirred for an additional 15 min, a suspension of 5.8 g (0.055 mole) of α-(methylthio)acetamide in 150 mL of methylene chloride was added. The mixture was stirred at -65° C. for 1 h. Triethylamine (5.6 g, 0.055 mole) was added and the solution was allowed to warm to room temperature. The reaction mixture was extracted with water and the organic layer dried over magnesium sulfate. The volume of the solution was reduced in vacuo to about 200 mL and the product crystallized as a yellow solid, m.p. 173.5°-174.5° C. Yield was 6.86 g (37.3%). was added The mixture was stirred at -65° C. for 1 h The reaction mixture was extracted with water the organic layer dried over magnesium sulfate the product crystallized as a yellow solid, m.p. 173.5°-174.5° C

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a cold (-70° C.) solution of 12.77 g (0.055 mole) of 2-amino-5-chlorobenzophenone in 300 ml of methylene chloride, under nitrogen atmosphere, was added 6.0 g (0.552 mole) of t-butylhypochlorite in 20 ml of methylene chloride. After an additional 15 min stirring period, a suspension of 5.8 g (0.055 mole) of α-(methylthio)acetamide in 150 ml of methylene chloride was added. The mixture was stirred at -65° C. for one hour. Triethylamine (5.6 g (0.055 mole)) was added and the solution was allowed to warm to room temperature. The reaction mixture was extracted with several portions of water and the organic layer dried over magnesium sulfate. The volume of solution was reduced in vacuo to about 200 ml and the product crystallized as a yellow solid, m.p. 173.5°-174.5° C. Yield was 6.86 g (37.3%). was added The mixture was stirred at -65° C. for one hour The reaction mixture was extracted with several portions of water the organic layer dried over magnesium sulfate the product crystallized as a yellow solid, m.p. 173.5°-174.5° C