Lithium borohydride → (6-Aminopyrimidin-4-yl)methanol
反応式
[NH2:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8](OC)=[O:9])[CH:3]=1.[Li+].[BH4-]>CO>[NH2:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([CH2:8][OH:9])[CH:3]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
To a stirred solution of methyl 6-aminopyrimidine-4-carboxylate (2.0 g, 13 mmol) in MeOH (20 mL) at 25° C., was added LiBH4 (0.85 g, 39 mmol). After addition, the resulting mixture was allowed to stir at 70° C. for 16 hours. TLC indicated the starting material was consumed completely at this point. Solvents were removed under reduced pressure and the residue was purified via chromatography column on silica gel eluting with a 5% gradient of methanol in dichloromethane to give the desired alcohol as pale yellow oil (1.0 g, 61% yield). LCMS (ESI) m/z: 126.1 [M+H+].
後処理
- additionAfter addition
- customwas consumed completely at this point
- customSolvents were removed under reduced pressure
- customthe residue was purified via chromatography column on silica gel eluting with a 5% gradient of methanol in dichloromethane
出典と根拠
- ORDレコード
- ord-4844b7b696b44e889a7cf08ae9bb0d30
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08697708B2
反応ノート
読み込み中…