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

HRID 258087노트

반응식

HRID 258087 반응식
[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]

참가 물질

7

반응물 5

HCID 962WaterHCID 8857Ethyl AcetateHCID 11430Potassium Carbonate2회HCID 27575041-(2-Chloroethyl)imidazole2회HCID 138011253-Phenyl-1H-pyrazolo[4,3-c]pyridine

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-6a4dc4231a9f47f289fae809b6ac5f97
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264576

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