Ethyl 4-cyano-4-(2,3-difluorophenyl)butanoate → 5-(2,3-Difluorophenyl)piperidin-2-one

HRID 334861노트

반응식

HRID 334861 반응식
[C:1]([CH:3]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:12]=1[F:18])[CH2:4][CH2:5][C:6](OCC)=[O:7])#[N:2]>[Ni].N>[F:18][C:12]1[C:13]([F:17])=[CH:14][CH:15]=[CH:16][C:11]=1[CH:3]1[CH2:1][NH:2][C:6](=[O:7])[CH2:5][CH2:4]1

참가 물질

4

반응물 1

HCID 68749022Ethyl 4-cyano-4-(2,3-difluorophenyl)butanoate

생성물 1

HCID 687484265-(2,3-Difluorophenyl)piperidin-2-one

시약·촉매·용매 2

HCID 935Nickel촉매HCID 222Ammonia용매

실험 절차

A mixture of ethyl 4-cyano-4-(2,3-difluorophenyl)butanoate (18.5 g, 73.1 mmol), Raney nickel (slurry in water, ca. 30 g), and ammonia (2.0 M in EtOH, 550 mL) was stirred vigorously under an atmosphere of hydrogen (ca. 1 atm) for 18 h. The reaction mixture was filtered through a pad of Celite®, washing with EtOH, and the filtrate was concentrated in vacuo to give a crude solid. Recrystallization from EtOAc afforded the title compound. MS: m/z=211.9 (M+1).

후처리

  1. filtrationThe reaction mixture was filtered through a pad of Celite®
  2. washwashing with EtOH
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto give a crude solid
  5. customRecrystallization from EtOAc

출처 및 근거

ORD 기록
ord-880b56644a274a97884e50196aaa5ac0
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883807B2

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