HCID 57633726、化合物 → HCID 57633720、化合物

HRID 2240884ノート

反応式

HRID 2240884 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]([CH2:15][C:16](=[CH2:21])[C:17]([O:19][CH3:20])=[O:18])[CH2:10][C:11]([F:14])([F:13])[F:12])=[CH:5][C:4]=1[C:22]([F:25])([F:24])[F:23])#[N:2]>CCOC(C)=O.[Pd]>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]([CH2:10][C:11]([F:14])([F:13])[F:12])[CH2:15][CH:16]([CH3:21])[C:17]([O:19][CH3:20])=[O:18])=[CH:5][C:4]=1[C:22]([F:23])([F:25])[F:24])#[N:2]

参加物

4

反応物 1

HCID 57633726HCID 57633726、化合物

生成物 1

HCID 57633720HCID 57633720、化合物収率 62.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

A suspension of 5% Pd/C (0.060 g) in EtOAc (3 mL) was stirred under an H2 atmosphere (balloon pressure) for 15 min. A solution of methyl 2-{[[4-cyano-3-(trifluoromethyl)phenyl](2,2,2-trifluoroethyl)amino]methyl}acrylate (0.090 g, 0.245 mmol) in EtOAc (3 mL) was added and the mixture stirred for 1 hr. The catalyst was filtered off and washed with EtOAc. The filtrate was concentrated and purified by silica gel chromatography to afford 0.056 g (62% yield) of the title compound: MS (ES) m/z 369 (M+1).

後処理

  1. stirringthe mixture stirred for 1 hr
  2. filtrationThe catalyst was filtered off
  3. washwashed with EtOAc
  4. concentrationThe filtrate was concentrated
  5. custompurified by silica gel chromatography

出典と根拠

ORDレコード
ord-8533fa2d3fca43ac8a3913f752502895
出典データセット
uspto-grants-2010_05
特許番号
US07723385B2

反応ノート

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