Hydrazine hydrate (1:1) → 5-Bromo-2-chloro-4-hydrazinylpyrimidine
反応式
[Br:1][C:2]1[C:3](Cl)=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1.O.[NH2:11][NH2:12]>C(O)C>[Br:1][C:2]1[C:3]([NH:11][NH2:12])=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1参加物
4
実験手順
A 500 mL round bottom flask was charged with 5-bromo-2,4-dichloropyrimidine (13.5 g, 59.2 mmol), hydrazine hydrate (8.8 mL, 181 mmol) and absolute ethanol (300 mL). The resulting solution was refluxed under N2 for 12 h. Work-up: the resulting crystalline solid was collected by filtration. The solid was washed with ethanol (100 mL), and dried to afford 17 g (quantitative) of the product as a yellow solid, which was used in the next step without further purification.
後処理
- temperatureThe resulting solution was refluxed under N2 for 12 h
- filtrationthe resulting crystalline solid was collected by filtration
- washThe solid was washed with ethanol (100 mL)
- customdried
出典と根拠
- ORDレコード
- ord-04047e1edb604a03b24f95968dc865e1
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08569300B2
反応ノート
読み込み中…