Diisobutylaluminum hydride → HCID 58574335、化合物
反応式
[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]=1参加物
4
実験手順
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+).
後処理
- 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
出典と根拠
- ORDレコード
- ord-2ff5f845aec9474f8c93eab479057b30
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772301B2
反応ノート
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