Dichloromethane → HCID 135702882、化合物

HRID 566341ノート

反応式

HRID 566341 の反応式
[NH2:1][C:2]1[N:6]([CH:7]([CH3:17])[CH2:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:5]=[C:4]([CH2:18][CH3:19])[C:3]=1[C:20]([NH2:22])=[O:21].[CH2:23]1[O:31][C:30]2[CH:29]=[CH:28][C:27]([CH2:32][C:33](OC)=O)=[CH:26][C:25]=2[O:24]1.ClCCl.C(=O)([O-])O.[Na+]>CC(C)([O-])C.[K+]>[CH2:23]1[O:31][C:30]2[CH:29]=[CH:28][C:27]([CH2:32][C:33]3[NH:22][C:20](=[O:21])[C:3]4[C:4]([CH2:18][CH3:19])=[N:5][N:6]([CH:7]([CH3:17])[CH2:8][CH2:9][CH2:10][C:11]5[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=5)[C:2]=4[N:1]=3)=[CH:26][C:25]=2[O:24]1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 266588Methyl 2-(1,3-dioxaindan-5-yl)acetateHCID 516892Sodium BicarbonateHCID 21266063HCID 21266063、化合物

生成物 1

HCID 135702882HCID 135702882、化合物収率 50%

試薬・触媒・溶媒 1

HCID 23665647Potassium tert-butoxide溶媒

実験手順

19 mg (0.063 mmol) of 5-amino-1-(1-methyl-4-phenyl-butyl)-3-ethyl-1H-pyrazole-4-carboxamide and 35 mg (0.180 mmol) of methyl 3,4-methylenedioxyphenylacetate are refluxed for 6 hours in 0.9 ml of 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 14 mg (48%) of a solid, Rf=0.64 (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-8b035a99bd384da4b51f3482b1539408
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…