Phosphorus oxychloride → 7-Chloropyrazolo[1,5-a]pyrimidine
反応式
[N:1]1[N:5]2[C:6](=O)[CH:7]=[CH:8][NH:9][C:4]2=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:13])=O.C(N(C(C)C)CC)(C)C>>[Cl:13][C:6]1[N:5]2[N:1]=[CH:2][CH:3]=[C:4]2[N:9]=[CH:8][CH:7]=1参加物
4
反応条件
- 温度
- 90 °C
実験手順
Pyrazolo[1,5-a]pyrimidin-7(4H)-one (0.50 g, 3.70 mmols), phosphorus oxychloride (0.88 ml, 9.62 mmols) and diisopropylethylamine (DIEA, 0.13 ml, 0.74 mmols) were mixed and stirred at 90° C. overnight. It was poured onto water/ice, extracted with dichloromethane and washed with brine. It was dried, filtered and concentrated in vacuum. It was purified by chromatography (Silica gel, Hexane/Ethyl acetate 9:1) to afford the expected compound (83 mg, 71%).
後処理
- additionIt was poured onto water/ice
- extractionextracted with dichloromethane
- washwashed with brine
- customIt was dried
- filtrationfiltered
- concentrationconcentrated in vacuum
- customIt was purified by chromatography (Silica gel, Hexane/Ethyl acetate 9:1)
出典と根拠
- ORDレコード
- ord-d07c9e370de242adad4af30969835e36
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09340547B2
反応ノート
読み込み中…