Sodium Hydroxide → 3-chloro-N-hydroxy-2,2-dimethylpropanamide

HRID 1995492ノート

反応式

HRID 1995492 の反応式
Cl.[NH2:2][OH:3].[OH-].[Na+].[Cl:6][CH2:7][C:8]([CH3:13])([CH3:12])[C:9](Cl)=[O:10]>O>[Cl:6][CH2:7][C:8]([CH3:13])([CH3:12])[C:9]([NH:2][OH:3])=[O:10]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 613453-Chloro-2,2-dimethylpropanoyl chlorideHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 37127643-chloro-N-hydroxy-2,2-dimethylpropanamide収率 40.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2630e9f77af749878337be963cbf2ab1
出典データセット
uspto-grants-1983_09
特許番号
US04405357

反応ノート

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