2-(3-CHLOROPHENYL)ACETAMIDE

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

実験手順: 7.32 g (55.9 mmol) of chlorocarbonylsulphenyl chloride and 7.90 g (46.6 mmol) of 2-(3-chlorophenyl)acetamide are stirred in 50 ml of toluene at 80° C. for 3 h. The crude product is reacted further without additional purification.

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

実験手順: (5-Chloro-2-nitrophenyl)acetamide (35.0 g, 30%) was prepared from 3-chloro phenyl acetamide (90.0 g, 0.53 mol) (obtained in step 1 above), conc. HNO3 (100 mL), conc. H2SO4 (156 mL) and dichloromethane (250 mL), by an analogous procedure to that described in preparation 1 (step 2). mp 115-116° C.; IR (KBr) 3329, 1693, 1504 cm-1 ; 1H NMR (CDCl3) δ 2.30 (s, 3H, CH3), 7.12 (d, J=8.4 Hz, 1H), 7.28 (s, 1H), 8.20 (d, J=8.4 Hz, 1H), 10.48 (brs, 1H, NH); Mass (m/z) 214 (M+.). that described in preparation 1 (step 2)

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

実験手順: (5-Chloro-2-nitrophenyl)acetamide (35.0 g, 30%) was prepared from 3-chloro phenyl acetamide (90.0 g, 0.53 mol) (obtained in step 1 above), conc. HNO3 (100 mL), conc. H2SO4 (156 mL) and dichloromethane (250 mL), by an analogous procedure to that described in preparation 1 (step 2). mp 115-116° C.; IR (KBr) 3329, 1693, 1504 cm-1 ; 1H NMR (CDCl3) δ 2.30 (s, 3H, CH3), 7.12 (d, J=8.4 Hz, 1H), 7.28 (s, 1H), 8.20 (d, J=8.4 Hz, 1H), 10.48 (brs, 1H, NH); Mass (m/z) 214 (M+.). that described in preparation 1 (step 2)

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

実験手順: 7.32 g (55.9 mmol) of chlorocarbonylsulphenyl chloride and 7.90 g (46.6 mmol) of 2-(3-chlorophenyl)acetamide are stirred in 50 ml of toluene at 80° C. for 3 h. The crude product is reacted further without additional purification.

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

実験手順: 7.32 g (55.9 mmol) of chlorocarbonylsulphenyl chloride and 7.90 g (46.6 mmol) of 2-(3-chlorophenyl)acetamide are stirred in 50 ml of toluene at 80° C. for 3 h. The crude product is reacted further without additional purification.

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

実験手順: (5-Chloro-2-nitrophenyl)acetamide (35.0 g, 30%) was prepared from 3-chloro phenyl acetamide (90.0 g, 0.53 mol) (obtained in step 1 above), conc. HNO3 (100 mL), conc. H2SO4 (156 mL) and dichloromethane (250 mL), by an analogous procedure to that described in preparation 1 (step 2). mp 115-116° C.; IR (KBr) 3329, 1693, 1504 cm-1 ; 1H NMR (CDCl3) δ 2.30 (s, 3H, CH3), 7.12 (d, J=8.4 Hz, 1H), 7.28 (s, 1H), 8.20 (d, J=8.4 Hz, 1H), 10.48 (brs, 1H, NH); Mass (m/z) 214 (M+.). that described in preparation 1 (step 2)

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

実験手順: 7.32 g (55.9 mmol) of chlorocarbonylsulphenyl chloride and 7.90 g (46.6 mmol) of 2-(3-chlorophenyl)acetamide are stirred in 50 ml of toluene at 80° C. for 3 h. The crude product is reacted further without additional purification.