N-chlorobenzamide

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A stream of gaseous chlorine in introduced at a speed of about 33 g/h into a suspension of 111 g of 99.5% pure benzamide (0.91 mol) in 700 ml of water maintained at a temperature of 15°-20° C. After 2 h and 15 min 75 g of chlorine (1.05 mol), controlled by weighing, have been absorbed. The mass is stirred for another 15 min at a temperature of 20° C., then the chlorinated product obtained is filtered off and is washed with water until the hydrochloric acid has disappeared. 140 g of N-chlorobenzamide (yield 98.9%) containing 21.87% of active chlorine, corresponding to a titer of 96%, are obtained. maintained at a temperature of 15°-20° C have been absorbed the chlorinated product obtained is filtered off is washed with water until the hydrochloric acid

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

実験手順: Dissolved in 200 ml of benzene were 18.5 g (0.12 mol) of benzenehydroxamic acid chloride synthesized in accordance with a known process [J.Org.Chem., 45, 3916 (1980)] and 10.0 g (0.12 mole) of 1-pentyne-3-ol, followed by the dropwise addition of 18 g (0.18 mol) of triethylamine under ice cooling. After they were reacted under reflux for 10 hours, the reaction mixture was washed with water and the organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby 5-(1-hydroxypropyl)-3-phenylisoxazole was obtained as colorless crystals. Analytical results of the crystals obtained: Yield: 19.3 g (79.7%). Melting point: 101°-102° C. After they were reacted under reflux for 10 hours the reaction mixture was washed with water the organic layer was dried over anhydrous sodium sulfate The solvent was distilled off under reduced pressure The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform)

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

実験手順: Dissolved in 200 ml of benzene were 18.5 g (0.12 mol) of benzenehydroxamic acid chloride synthesized in accordance with a known process [J. Org. Chem., 45, 3916 (1980)] and 10.0 g (0.12 mole) of 1-pentyne-3-ol, followed by the dropwise addition of 18 g (0.18 mol) of triethylamine under ice cooling. After they were reacted under reflux for 10 hours, the reaction mixture was washed with water and the organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby 5-(1-hydroxypropyl)-3-phenylisoxazole was obtained as colorless crystals. After they were reacted under reflux for 10 hours the reaction mixture was washed with water the organic layer was dried over anhydrous sodium sulfate The solvent was distilled off under reduced pressure The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform)

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

実験手順: Dissolved in 200 ml of benzene were 18.5 g (0.12 mol) of benzenehydroxamic acid chloride synthesized in accordance with a known process [J.Org.Chem., 45, 3916 (1980)] and 10.0 g (0.12 mole) of 1-pentyne-3-ol, followed by the dropwise addition of 18 g (0.18 mol) of triethylamine under ice cooling. After they were reacted under reflux for 10 hours, the reaction mixture was washed with water and the organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. .The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby 5-(1-hydroxypropyl)-3-phenylisoxazole was obtained as colorless crystals. After they were reacted under reflux for 10 hours the reaction mixture was washed with water the organic layer was dried over anhydrous sodium sulfate The solvent was distilled off under reduced pressure .The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform)