Hydrochloric Acid → 5-Chloro-1H-pyrazolo(4,3-d)pyrimidine
反応式
Cl.[Cl:2][C:3]1[N:4]=[CH:5][C:6]2[N:11](C(=O)C)[N:10]=[CH:9][C:7]=2[N:8]=1>O1CCCC1>[Cl:2][C:3]1[N:4]=[CH:5][C:6]2[NH:11][N:10]=[CH:9][C:7]=2[N:8]=1参加物
4
実験手順
Hydrochloric acid (70 mL, 8%) was added dropwise to a solution of 1-[5-chloro-1H-pyrazolo[4,3-d]pyrimidin-1-yl]ethan-1-one (7 g, 33.83 mmol, 1.00 equiv, 95%) in tetrahydrofuran (70 mL) at 50° C. The resulting solution was refluxed for 30 min and then extracted with 2×100 mL of ethyl acetate. The organic layers were combined, dried over anhydrous sodium sulfate and concentrated under vacuum to give 2.5 g (45%) of 5-chloro-1H-pyrazolo[4,3-d]pyrimidine as a white solid.
後処理
- temperatureThe resulting solution was refluxed for 30 min
- extractionextracted with 2×100 mL of ethyl acetate
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-64f3d0304fd8400d87ba03b2ba0b13f8
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653089B2
反応ノート
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