Hydrazine → Hydrazinecarboxylic acid, phenyl ester
반응식
[NH2:1][NH2:2].Cl[C:4]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:5]>CCOCC>[NH:1]([C:4]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:5])[NH2:2]참가 물질
4
실험 절차
To a solution of hydrazine (0.83 mL, 26 mmol) in ether was added phenyl chloroformate (0.92 mL, 7.4 mmol) at −20° C. The solution was stirred for 1 h, removed solid by filtration, and filtrate was concentrated to give phenyl hydrazinecarboxylate. To phenyl hydrazinecarboxylate was added compound 2b (1.2 g, 5.2 mmol), THF (20 mL), and DIPEA (1.5 mL) and the solution was stirred for 1 h. Partitioned reaction between sat. aq. NaHCO3 and CH2Cl2, dried (MgSO4), filtered, and concentrated to yield compound 81a (400 mg, 22%).
후처리
- customremoved solid
- filtrationby filtration, and filtrate
- concentrationwas concentrated
출처 및 근거
- ORD 기록
- ord-46c70f04a18b48ae8e42b25d80a6957d
- 출처 데이터셋
- uspto-grants-2013_04
- 특허 번호
- US08415353B2
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