Acetic Anhydride → Acetylamphetamine

HRID 1065203

반응식

HRID 1065203 반응식
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

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 222898Amphedrine

생성물 1

HCID 26660Acetylamphetamine

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-08760780cc7c4aeebd9fa73e0d981d98
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04329281

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