反应详情

A stirred solution of 28.0 grams (0.40 mole) of hydroxylamine hydrochloride in 60 ml of water was cooled to 0° and a solution of 16.0 grams (0.40 mole) of sodium hydroxide in 40 ml of water was added dropwise while maintaining the temperature of the reaction mixture at 0°-5°. Upon completion of addition 31.0 grams (0.20 mole) of 3-chloro-2,2-dimethylpropionyl chloride was added dropwise during a 45-minute period while maintaining the temperature of the reaction mixture at -3° to -5°. Upon completion of addition the reaction mixture was maintained at 5° for one hour, then was allowed to warm to ambient temperature where it was stirred for 16 hours. A white solid precipitate was collected by filtration and air-dried. The dried solid was recrystallized from ethanol-water to give 12.4 grams of 3-chloro-N-hydroxy-2,2-dimethylpropanamide; mp 148°-151°, decomposes.

1. temperaturewhile maintaining the temperature of the reaction mixture at 0°-5°
2. additionwas added dropwise during a 45-minute period
3. temperaturewhile maintaining the temperature of the reaction mixture at -3° to -5°
4. additionUpon completion of addition the reaction mixture
5. temperaturewas maintained at 5° for one hour
6. filtrationA white solid precipitate was collected by filtration
7. customair-dried
8. customThe dried solid was recrystallized from ethanol-water