Acetic Anhydride → 1-[2-(Propan-2-yl)pyrazolo[1,5-a]pyridin-3-yl]ethan-1-one
반응식
[CH:1]([C:4]1[CH:12]=[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][N:6]2[N:5]=1)([CH3:3])[CH3:2].[C:13](OC(=O)C)(=[O:15])[CH3:14]>S(=O)(=O)(O)O.[OH-].[K+]>[C:13]([C:12]1[C:4]([CH:1]([CH3:3])[CH3:2])=[N:5][N:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=12)(=[O:15])[CH3:14]참가 물질
5
실험 절차
A mixture of 4.2g of 2-isopropylpyrazolo[1,5-a]-pyridine, 10.2g of acetic anhydride and 2-3 drops of concentrated sulfuric acid was refluxed for 7 hr. After cooling, the mixture was added to 200 ml of 4M potassium hydroxide solution and stirred for 1 hr. The solution was extracted with chloroform and the chloroform solution was dried over sodium sulfate. The dried chloroform solution was concentrated and the residue was columnchromatographed over alumina to isolate objective product. Recrystallization from n-hexane gave 4.3g of colorless needles, mp 74° C. Yield 67%.
후처리
- temperaturewas refluxed for 7 hr
- temperatureAfter cooling
- extractionThe solution was extracted with chloroform
- dry with materialthe chloroform solution was dried over sodium sulfate
- concentrationThe dried chloroform solution was concentrated
- customto isolate objective product
- customRecrystallization from n-hexane
출처 및 근거
- ORD 기록
- ord-7501d1dc34534a46a42280ac97b4d82c
- 출처 데이터셋
- uspto-grants-1978_06
- 특허 번호
- US04097483
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