Acetic Anhydride → Acetylamphetamine

HRID 1065203

反応式

HRID 1065203 の反応式
S(O)(O)(=O)=O.[NH2:6][CH:7]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH3:8].[OH-].[Na+].[C:18](OC(=O)C)(=[O:20])[CH3:19]>O>[CH3:8][CH:7]([NH:6][C:18](=[O:20])[CH3:19])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 222898Amphedrine

生成物 1

HCID 26660Acetylamphetamine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Seventy three and six tenths g (0.2 moles) of rac. amphetamine sulfate was suspended in 150 ml of water and to the stirred suspension, a solution of twenty g (0.5 moles) of sodium hydroxide in 200 ml of water was added. The liberated oil was collected by three extractions with 200-ml portions of toluene. The combined extracts were dried over anhydrous K2CO3, then the drying agent removed by filtration. To the filtrate, 100 ml of acetic anhydride (1.0 mole) was added in portions and the resulting solution refluxed for two hours. The toluene, excess anhydride and acetic acid were distilled in the rotary evaporator and the residual oil distilled in a simple Claisen still collecting the fractions that boiled at 120°-126°/7 mm, yield 63.3 g (89%) of a colorless oil that spontaneously set to a mass of crystals, mp 91°-93°.

後処理

  1. customThe liberated oil was collected by three extractions with 200-ml portions of toluene
  2. dry with materialThe combined extracts were dried over anhydrous K2CO3
  3. customthe drying agent removed by filtration
  4. temperaturethe resulting solution refluxed for two hours
  5. distillationThe toluene, excess anhydride and acetic acid were distilled in the rotary evaporator
  6. distillationthe residual oil distilled in a simple Claisen
  7. customstill collecting the fractions that boiled at 120°-126°/7 mm, yield 63.3 g (89%) of a colorless oil

出典と根拠

ORDレコード
ord-08760780cc7c4aeebd9fa73e0d981d98
出典データセット
uspto-grants-1982_05
特許番号
US04329281

関連ノート

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