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

HRID 914815

反応式

HRID 914815 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5213051-Chloroethyl chloroformate溶媒

実験手順

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).

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, 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

出典と根拠

ORDレコード
ord-73d21e929b3845a39e8174d64c041f64
出典データセット
uspto-grants-2007_09
特許番号
US07265108B2

関連ノート

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