Diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate → Ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylate

HRID 71110

반응식

HRID 71110 반응식
[C:1]([CH2:3][CH2:4][C:5]([C:16]1[CH:21]=[CH:20][C:19]([F:22])=[C:18]([F:23])[CH:17]=1)([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6](OCC)=[O:7])#[N:2]>[Co].N>[F:23][C:18]1[CH:17]=[C:16]([C:5]2([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:4][CH2:3][CH2:1][NH:2][C:6]2=[O:7])[CH:21]=[CH:20][C:19]=1[F:22]

참가 물질

4

반응물 1

HCID 66608241Diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate

생성물 1

HCID 66607999Ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylate수율 79.3%

시약·촉매·용매 2

HCID 104730Cobalt촉매HCID 222Ammonia용매

실험 절차

A mixture of diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate (15.2 g), Raney cobalt (75 g) and ammonia (2M ethanol solution, 150 mL) was stirred at room temperature for 3 days under a hydrogen atmosphere. The insoluble material was filtered off through celite, and the filtrate was concentrated under reduced pressure. The residue was washed with diisopropylether to give the title compound (10.5 g).

후처리

  1. filtrationThe insoluble material was filtered off through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. washThe residue was washed with diisopropylether

출처 및 근거

ORD 기록
ord-42390afab45e45948b53e8b96a946d2e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822699B2

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