Hydrazine hydrate (1:1) → Tert-butyl 2-chloro-6-hydrazinoisonicotinate
反応式
[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]参加物
4
反応条件
- 温度
- 75 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-d67b05ebaec347e0ab1353b2aaa53272
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09238647B2
反応ノート
読み込み中…