HCID 57714115、化合物 → HCID 57714122、化合物

HRID 1984255ノート

反応式

HRID 1984255 の反応式
[CH3:1][C:2]([CH3:23])([CH3:22])[CH2:3][N:4]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]#[CH:21])=[CH:16][CH:15]=1)[C:5]1[CH:10]=[CH:9][N:8]=[C:7]([C:11]#[N:12])[N:6]=1>CCO.[Pd]>[CH3:1][C:2]([CH3:22])([CH3:23])[CH2:3][N:4]([CH2:13][C:14]1[CH:15]=[CH:16][C:17]([CH2:20][CH3:21])=[CH:18][CH:19]=1)[C:5]1[CH:10]=[CH:9][N:8]=[C:7]([C:11]#[N:12])[N:6]=1

参加物

4

反応物 1

HCID 57714115HCID 57714115、化合物

生成物 1

HCID 57714122HCID 57714122、化合物収率 112%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

4-[(2,2-Dimethyl-propyl)-(4-ethynyl-benzyl)-amino]-pyrimidine-2-carbonitrile (47 mg, 0.11 mmoles) is dissolved in 5 ml of EtOH and 10% Pd—C (5 mg) is added at rt. The mixture is stirred under hydrogen at rt for overnight and is filtered through a pad of Celite which is washed with EtOH. The filtrate is concentrated and the crude product is purified by silica gel column chromatography to give 38 mg of desired 4-[(2,2-dimethyl-propyl)-(4-ethyl-benzyl)-amino]-pyrimidine-2-carbonitrile in 77% yield.

後処理

  1. filtrationis filtered through a pad of Celite which
  2. washis washed with EtOH
  3. concentrationThe filtrate is concentrated
  4. customthe crude product is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-262ef51fc33545579ea0469bba51db3a
出典データセット
uspto-grants-2009_06
特許番号
US07544688B2

反応ノート

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