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

HRID 606179ノート

反応式

HRID 606179 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5213051-Chloroethyl chloroformate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d97aa03472264ef8aed64a5602eada4f
出典データセット
uspto-grants-2011_03
特許番号
US07915274B2

反応ノート

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