1,2-Dichloroethane → 1-(Piperidin-4-yl)-2-[2-(trifluoromethyl)phenyl)ethanone hydrochloride

HRID 606179노트

반응식

HRID 606179 반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[O:26])[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([F:25])([F:24])[F:23])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:27]CCCl>ClC(OC(Cl)C)=O>[ClH:27].[NH:8]1[CH2:9][CH2:10][CH:11]([C:14](=[O:26])[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([F:24])([F:25])[F:23])[CH2:12][CH2:13]1

참가 물질

4

반응물 2

HCID 111,2-DichloroethaneHCID 222479231-(1-Benzylpiperidin-4-yl)-2-[2-(trifluoromethyl)phenyl]ethanone

생성물 1

HCID 222484771-(Piperidin-4-yl)-2-[2-(trifluoromethyl)phenyl)ethanone hydrochloride수율 83%

시약·촉매·용매 1

HCID 5213051-Chloroethyl chloroformate용매

실험 절차

After dissolving 1.30 g of 1-(1-benzylpiperidin-4-yl)-2-[2-(trifluoromethyl)phenyl]ethanone in 10 ml of 1,2-dichloroethane, 0.58 ml of 1-chloroethyl chloroformate was added while stirring at room temperature and the mixture was heated to reflux for 1 hour. The solvent was distilled off under reduced pressure, 10 ml of methanol was added to the residue and heating to reflux was continued for 30 minutes. The solvent was distilled off under reduced pressure, ethyl acetate/n-hexane was added to the residue and the precipitate was filtered out to obtain the title compound (916 mg, 83% 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, 10 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/n-hexane
  9. additionwas added to the residue
  10. filtrationthe precipitate was filtered out

출처 및 근거

ORD 기록
ord-d97aa03472264ef8aed64a5602eada4f
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915274B2

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