Diisobutylaluminum hydride → HCID 58574335, 화합물
반응식
[Br:1][C:2]1[CH:16]=[CH:15][N:5]2[C:6](=[O:14])[C:7]([C:10](OC)=[O:11])=[CH:8][N:9]=[C:4]2[CH:3]=1.CC(C[AlH]CC(C)C)C>C1COCC1>[Br:1][C:2]1[CH:16]=[CH:15][N:5]2[C:6](=[O:14])[C:7]([CH2:10][OH:11])=[CH:8][N:9]=[C:4]2[CH:3]=1참가 물질
4
실험 절차
To a solution of methyl 8-bromo-4-oxo-4H-pyrido[1,2-a]pyrimidine-3-carboxylate (1 g, 3.5 mmol, 1 equiv) in anhydrous THF (25 mL) was added DIBAL-H (5 mL) at 0° C. dropwise. After stirring for 1 h, the reaction mixture was quenched with saturated NH4Cl. The solution was extracted with ethyl acetate (3×150 mL). The combined organic layers were dried over Na2SO4 and concentrated to give the crude product. The crude was purified by column chromatography to give 145 mg of the desired product. MS (ESI): 255, 257 (MH+).
후처리
- customthe reaction mixture was quenched with saturated NH4Cl
- extractionThe solution was extracted with ethyl acetate (3×150 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- concentrationconcentrated
- customto give the crude product
- customThe crude was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-2ff5f845aec9474f8c93eab479057b30
- 출처 데이터셋
- uspto-grants-2014_07
- 특허 번호
- US08772301B2
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