Benzeneacetic acid, 3,4-dimethoxy-, methyl ester → HCID 136132162、化合物

HRID 566356ノート

反応式

HRID 566356 の反応式
[NH2:1][C:2]1[N:6]([CH:7]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH2:8][CH2:9][CH3:10])[N:5]=[C:4]([CH3:17])[C:3]=1[C:18]([NH2:20])=[O:19].[CH3:21][O:22][C:23]1[CH:24]=[C:25]([CH2:31][C:32](OC)=O)[CH:26]=[CH:27][C:28]=1[O:29][CH3:30].CC(C)([O-])C.[K+].C(=O)([O-])O.[Na+]>ClCCl>[CH3:21][O:22][C:23]1[CH:24]=[C:25]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[CH2:31][C:32]1[NH:20][C:18](=[O:19])[C:3]2[C:4]([CH3:17])=[N:5][N:6]([CH:7]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH2:8][CH2:9][CH3:10])[C:2]=2[N:1]=1

参加物

6

反応物 4

HCID 85213Benzeneacetic acid, 3,4-dimethoxy-, methyl esterHCID 516892Sodium BicarbonateHCID 23665647Potassium tert-butoxideHCID 59932332HCID 59932332、化合物

生成物 1

HCID 136132162HCID 136132162、化合物収率 26%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

6 mg (0.021 mmol) of 5-amino-3-methyl-1-(4-decyl)-1H-pyrazole-4-carboxamide and 20 mg (0.095 mmol) of methyl 3,4-dimethoxyphenylacetate are refluxed for 6 hours in 0.3 ml of a 0.5M ethanolic potassium tert-butoxide solution. After dichloromethane and saturated aqueous sodium hydrogen carbonate solution have been added, the phases are separated. Purification by chromatography gives 2.4 mg (26%) of a solid, Rf=0.66 (dichloromethane/methanol=15:1).

後処理

  1. customthe phases are separated
  2. customPurification by chromatography

出典と根拠

ORDレコード
ord-530deab19a5d4f1898329c4b2d973aab
出典データセット
uspto-grants-2001_01
特許番号
US06174884B1

反応ノート

読み込み中…