반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[CH2:9][CH2:10][CH2:11][N:12]1C(=O)C2C(=CC=CC=2)C1=O.C(O)C.NN>>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[CH2:9][CH2:10][CH2:11][NH2:12]참가 물질
4
실험 절차
A 10 g (34.4 mmole) sample of the title compound of Example 33 was refluxed for 2 hours in 150 ml of ethanol containing 1.2 g (36.7 mmole) of 97% hydrazine. After concentrating the solution, the white crystalline residue was mixed with 100 ml of 10% NaOH and 100 ml of ether. The aqueous phase was separated and extracted with another 100 ml portion of ether. The combined ether extracts were than washed with water, dried over MgSO4 and stripped of all solvent under reduced pressure to yield 3.3 g (59%) of the product as an oil. This material was used without further purification.
후처리
- concentrationAfter concentrating the solution
- additionthe white crystalline residue was mixed with 100 ml of 10% NaOH and 100 ml of ether
- customThe aqueous phase was separated
- extractionextracted with another 100 ml portion of ether
- washthan washed with water
- dry with materialdried over MgSO4
출처 및 근거
- ORD 기록
- ord-59ee8f90580b491d9685262ca4315869
- 출처 데이터셋
- uspto-grants-1988_02
- 특허 번호
- US04727189
연결된 노트
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