Water → 1-[2-(1H-Imidazoyl)ethyl]-3-phenyl-1H-pyrazolo[4,3-c]pyridine

HRID 487590ノート

反応式

HRID 487590 の反応式
[C:1]1([C:7]2[C:11]3[CH:12]=[N:13][CH:14]=[CH:15][C:10]=3[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClCC[N:19]1[CH:23]=[CH:22][N:21]=[CH:20]1.[C:24]([O-:27])([O-])=O.[K+].[K+].O.[C:31](OCC)(=O)[CH3:32]>CN(C)C=O>[NH:21]1[CH:22]=[CH:23][N:19]=[C:20]1[C:24]([CH2:31][CH2:32][N:9]1[C:10]2[CH:15]=[CH:14][N:13]=[CH:12][C:11]=2[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8]1)=[O:27]

参加物

7

反応物 5

HCID 962WaterHCID 8857Ethyl AcetateHCID 11430Potassium Carbonate2 回HCID 27575041-(2-Chloroethyl)imidazole2 回HCID 138011253-Phenyl-1H-pyrazolo[4,3-c]pyridine

生成物 1

HCID 199304931-[2-(1H-Imidazoyl)ethyl]-3-phenyl-1H-pyrazolo[4,3-c]pyridine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-Phenyl-1H-pyrazolo[4,3-c]pyridine (2.93 g) was suspended in 30 ml of N,N-dimethylformamide to which 1-(2-chloroethyl)imidazole (2.15 g) and K2CO3 (2.3 g) had been added. This mixture was stirred and warmed at 90° for 2 hours and then an additional 0.20 g of 1-(2-chloroethyl)imidazole and 0.2 g of K2CO3 were added. After an additional 45 minutes, the reaction mixture was distributed between H2O and ethyl acetate and the organic phase was washed with water. Evaporation and trituration with ether gave 2.15 g of product after recrystallization from CH2Cl2 -pentane, mp 123°-125°.

後処理

  1. additionhad been added
  2. temperaturewarmed at 90° for 2 hours
  3. washthe organic phase was washed with water
  4. customEvaporation and trituration with ether

出典と根拠

ORDレコード
ord-8d732942e172422ab0d065635f8b7c2f
出典データセット
uspto-grants-1994_03
特許番号
US05296491

反応ノート

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