1-Chloroethyl chloroformate → 4-Propenylidenepiperidine hydrochloride

HRID 1737432

반응식

HRID 1737432 반응식
C([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][CH2:15][CH3:16])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:17]C(OC(Cl)C)=O>ClC(Cl)C>[ClH:17].[CH:14](=[C:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1)[CH:15]=[CH2:16]

참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 149666551-Benzyl-4-propylidenepiperidine

생성물 1

HCID 867520404-Propenylidenepiperidine hydrochloride수율 110.4%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

There was dissolved 4.5 g (21 mmol) of 1-benzyl-4-propylidenepiperidine in 20 ml of dichloroethane and thereto 2.8 ml (25 mmol) of 1-chloroethyl chloroformate was added dropwise under cooling with ice. The reaction solution was stirred at room temperature for 30 minutes and then refluxed with heating for 30 minutes. The reaction solution was concentrated to 10 ml by removing the solvent under reduced pressure, and thereto was added 60 ml of methanol and the obtained mixture was refluxed with heating for 12 hours. The solvent was removed under reduced pressure to obtain 3.7 g of the titled compound.

후처리

  1. temperatureunder cooling with ice
  2. temperaturerefluxed
  3. temperaturewith heating for 30 minutes
  4. concentrationThe reaction solution was concentrated to 10 ml
  5. customby removing the solvent under reduced pressure
  6. additionwas added 60 ml of methanol
  7. temperaturethe obtained mixture was refluxed
  8. temperaturewith heating for 12 hours
  9. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-5f814a9447154d57b213afbfc5b09403
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962476

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