1-Chloroethyl chloroformate → 4-Benzylidenepiperidine hydrochloride

HRID 861946

反応式

HRID 861946 の反応式
C([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:21]C(OC(Cl)C)=O>ClC(Cl)C>[ClH:21].[CH:14](=[C:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

4

反応物 2

HCID 5213051-Chloroethyl chloroformateHCID 218433641-Benzyl-4-benzylidenepiperidine

生成物 1

HCID 185390104-Benzylidenepiperidine hydrochloride収率 42.7%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

There was dissolved 24.6 g (96 mmol) of 1-benzyl-4-benzylidenepiperidine in 200 ml of dichloroethane and thereto 11.1 ml (102 mmol) of 1-chloroethyl chloroformate was added dropwise under cooling with ice. The reaction solution was refluxed with heating for 30 minutes and then stirred at room temperature for 1.5 hours. The reaction solution was concentrated to 80 ml by removing the solvent under reduced pressure, thereto was added 200 ml of methanol and the obtained mixture was refluxed with heating for 12 hours. The solvent was removed under reduced pressure and to the obtained residue was added 100 ml of isopropyl ether and the precipitate was separated by filtration to obtain 8.6 g of the titled compound.

後処理

  1. temperatureunder cooling with ice
  2. temperatureThe reaction solution was refluxed
  3. temperaturewith heating for 30 minutes
  4. concentrationThe reaction solution was concentrated to 80 ml
  5. customby removing the solvent under reduced pressure
  6. additionwas added 200 ml of methanol
  7. temperaturethe obtained mixture was refluxed
  8. temperaturewith heating for 12 hours
  9. customThe solvent was removed under reduced pressure and to the obtained residue
  10. additionwas added 100 ml of isopropyl ether
  11. customthe precipitate was separated by filtration

出典と根拠

ORDレコード
ord-28b37068acdc4ae4a559829bf9f32b71
出典データセット
uspto-grants-1998_02
特許番号
US05716969

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