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

HRID 71110

反応式

HRID 71110 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 104730Cobalt触媒HCID 222Ammonia溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-42390afab45e45948b53e8b96a946d2e
出典データセット
uspto-grants-2014_09
特許番号
US08822699B2

関連ノート

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