反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 3-[8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazin-3-yl]-2-methyl-imidazo[1,2-a]pyridine-8-carboxaldehyde (0.33 g, 0.89 mmol) in CH3OH 910 ml) is treated with NaBH4 (37 mg, 0.98 mmol), and stirred at RT for 30 min. It is quenched with sat. NH4Cl (5 mL), the organic solvent is removed in vacuo, and the residue is diluted with H2O (10 mL) ppm. The aqueous layer is extracted with EtOAC (2×30 mL); the combined organic layers is dried with Na2SO4; filtered and concentrated to give the title compound (0.29 g, 0.78 mmol, 87%). 1H NMR (CDCl3): δ. 0.90 (t, J=7.0 Hz, 3H), 0.91 (t, J=7.0 Hz, 3H), 1.78-1.98 (m, 4H), 2.42 (s, 3H), 2.43 (s, 3H), 2.45 (s, 3H), 3.36-3.42 (m, 1H), 4.39 (bs, 1H), 5.11 (s, 2H), 6.73 (d, J=5.7 Hz, 1H), 6.73 (s, 1H), 7.17 (d, J=6.6 Hz, 1H), 7.46 (d, J=6.6 Hz, 1H) ppm. ES-MS (m/z): calcd for C22H27N5O (M+H)+: 378.5. found: 378.3.
WORKUP
后处理
- customIt is quenched with sat. NH4Cl (5 mL)
- customthe organic solvent is removed in vacuo
- additionthe residue is diluted with H2O (10 mL) ppm
- extractionThe aqueous layer is extracted with EtOAC (2×30 mL)
- dry with materialthe combined organic layers is dried with Na2SO4
- filtrationfiltered
- concentrationconcentrated