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

HRID 49779

반응식

HRID 49779 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e12882cfc33742e9af733bf1dc0f1f80
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710043B1

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