1,2-Dichloroethane → 2-(2-Fluorophenyl)-1-(piperidin-4-yl)ethanone hydrochloride

HRID 890027

반응식

HRID 890027 반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[O:23])[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[F:22])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:24]CCCl>ClC(OC(Cl)C)=O>[ClH:24].[F:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[CH2:15][C:14]([CH:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)=[O:23]

참가 물질

4

반응물 2

HCID 111,2-DichloroethaneHCID 222479931-(1-Benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanone

생성물 1

HCID 222481242-(2-Fluorophenyl)-1-(piperidin-4-yl)ethanone hydrochloride수율 92%

시약·촉매·용매 1

HCID 5213051-Chloroethyl chloroformate용매

실험 절차

After dissolving 1.27 g of 1-(1-benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanone in 8 ml of 1,2-dichloroethane, 0.53 ml of 1-chloroethyl chloroformate was added while stirring on ice, and the mixture was heated to reflux for 1 hour. The solvent was distilled off under reduced pressure, 8 ml of methanol was added to the residue, and heating to reflux was continued for 40 minutes. The solvent was distilled off under reduced pressure, ethyl acetate was added to the residue, and the precipitate was filtered out to obtain the title compound (970 mg, 92% yield).

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 1 hour
  4. distillationThe solvent was distilled off under reduced pressure, 8 ml of methanol
  5. additionwas added to the residue
  6. temperatureheating
  7. temperatureto reflux
  8. distillationThe solvent was distilled off under reduced pressure, ethyl acetate
  9. additionwas added to the residue
  10. filtrationthe precipitate was filtered out

출처 및 근거

ORD 기록
ord-90d6f9cbc5ce46b78e3bf3373bca84a1
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995144B2

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