Hydrochloric Acid → 3H-1,2-dihydro-1-pyrrolizinone

HRID 52194

반응식

HRID 52194 반응식
[C:1]([CH2:3][CH2:4][N:5]1[CH:9]=[CH:8][CH:7]=[CH:6]1)#N.Cl.CC[O:13]CC>>[C:1]1(=[O:13])[C:9]2[N:5]([CH:6]=[CH:7][CH:8]=2)[CH2:4][CH2:3]1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 965273-(Pyrrol-1-yl)propiononitrile

생성물 1

HCID 973473H-1,2-dihydro-1-pyrrolizinone수율 65%

실험 절차

To a solution of 10 g N-cyanoethylpyrrole in 100 ml ether was added 2.5 g ZnCI2. Dried HCl was passed into the mixture at 5°-10° C. After 2 hours, the reaction mixture was allowed to stand at room temperature for 4 hours. Removed the solvent by suction, 20%. Aqueous NaOH was added until pH 3. The mixture was stirred at 80°-90° C. for 2 hours. Extracted with methylene chloride, dried over Na2SO4, evaporated the solvent, 8 g yellow solid was obtained. The crude product was crystallized from petroleum ether, 6.5 g compound (1) was obtained, as white crystals, mp 53°-54.5° C., yield 65%.

후처리

  1. customwas passed into the mixture at 5°-10° C
  2. waitto stand at room temperature for 4 hours
  3. customRemoved the solvent by suction, 20%
  4. additionAqueous NaOH was added until pH 3
  5. extractionExtracted with methylene chloride
  6. dry with materialdried over Na2SO4
  7. customevaporated the solvent

출처 및 근거

ORD 기록
ord-4e56c64ca6304ac28913658aab4ebe4a
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616604

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