Water → 1-Acetyl-4-(4-fluorophenoxycarbonylamino)piperidine

HRID 49779

反応式

HRID 49779 の反応式
Cl.[C:2]([N:5]1[CH2:10][CH2:9][CH:8]([NH2:11])[CH2:7][CH2:6]1)(=[O:4])[CH3:3].N1C=CC=CC=1.Cl[C:19]([O:21][C:22]1[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=1)=[O:20].O>ClCCl.C(OCC)(=O)C>[C:2]([N:5]1[CH2:10][CH2:9][CH:8]([NH:11][C:19]([O:21][C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)=[O:20])[CH2:7][CH2:6]1)(=[O:4])[CH3:3]

参加物

7

反応物 4

HCID 962WaterHCID 1049PyridineHCID 27332564-Fluorophenyl chloroformateHCID 172216421-Acetyl-4-aminopiperidine hydrochloride

生成物 1

HCID 98171611-Acetyl-4-(4-fluorophenoxycarbonylamino)piperidine

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of 1-acetyl-4-aminopiperidine hydrochloride (0.4 g) in dichloromethane (5 ml) were added in turn pyridine (0.54 ml) and 4-fluorophenyl chloroformate (0.29 ml) at 0° C. The mixture was allowed to warm to ambient temperature and stirred for 1 hour, which was taken up into a mixture of water and ethyl acetate. The separated organic layer was washed in turn with hydrochloric acid (1N), aqueous sodium hydrogen carbonate, and brine, and dried over magnesium sulfate. Evaporation under reduced pressure gave a residue, which was triturated with diisopropyl ether to give 1-acetyl-4-(4-fluorophenoxycarbonylamino)piperidine (347 mg).

後処理

  1. washThe separated organic layer was washed in turn with hydrochloric acid (1N), aqueous sodium hydrogen carbonate, and brine
  2. dry with materialdried over magnesium sulfate
  3. customEvaporation under reduced pressure
  4. customgave a residue, which
  5. customwas triturated with diisopropyl ether

出典と根拠

ORDレコード
ord-e12882cfc33742e9af733bf1dc0f1f80
出典データセット
uspto-grants-2004_03
特許番号
US06710043B1

関連ノート

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