Hydrazine hydrate (1:1) → Tert-butyl 2-chloro-6-hydrazinoisonicotinate
반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[C:13](Cl)[N:14]=1)[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6].O.[NH2:17][NH2:18]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[C:13]([NH:17][NH2:18])[N:14]=1)[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6]참가 물질
4
반응 조건
- 온도
- 75 °C
실험 절차
To a solution of tert-butyl 2,6-dichloroisonicotinate (11.0 g, 44.3 mmol) in ethanol (222 mL) was added hydrazine hydrate (6.46 mL, 133 mmol). The mixture was heated 75° C. After 18 h, the mixture was cooled to ambient temperature. The mixture was concentrate down to half of the volume. The solid crashed out was filtered off and the filtrate was concentrated to dryness: LC-MS [M+1]=244.1.
후처리
- temperaturethe mixture was cooled to ambient temperature
- concentrationThe mixture was concentrate down to half of the volume
- filtrationThe solid crashed out was filtered off
- concentrationthe filtrate was concentrated to dryness
출처 및 근거
- ORD 기록
- ord-d67b05ebaec347e0ab1353b2aaa53272
- 출처 데이터셋
- uspto-grants-2016_01
- 특허 번호
- US09238647B2
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