1-Chloroethyl chloroformate → 4-Propenylidenepiperidine hydrochloride

HRID 1737432ノート

反応式

HRID 1737432 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 867520404-Propenylidenepiperidine hydrochloride収率 110.4%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5f814a9447154d57b213afbfc5b09403
出典データセット
uspto-grants-1999_10
特許番号
US05962476

反応ノート

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