Lithium borohydride → (6-Aminopyrimidin-4-yl)methanol
반응식
[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]=1참가 물질
4
반응 조건
- 온도
- 70 °C
실험 절차
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+].
후처리
- 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
출처 및 근거
- ORD 기록
- ord-4844b7b696b44e889a7cf08ae9bb0d30
- 출처 데이터셋
- uspto-grants-2014_04
- 특허 번호
- US08697708B2
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