HRID1158466
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
CONDITIONS
反应条件
- 温度
- 2.5 °C
PROCEDURE
实验过程
To a suspension of 5-bromo-2-methoxy-benzaldehyde (7.00 g, 32.2 mmol) in MeOH (40 mL), cooled to 0 to 5° C., is added NaBH4 (1.40 g, 35.4 mmol). After stirring for 1 h, the mixture is poured into ice-water, followed by extraction with AcOEt. The combined organics are washed with brine, dried (Na2SO4) and concentrated to give the title product as off-white solid. TLC, Rf (hexane/AcOEt 3:1)=0.19. 1H-NMR (CDCl3): δ 2.24 (m, 2H), 3.88 (s, 3H), 4.68 (d, 2H), 6.79 (dd, 1H), 7.41 (dd, 1H), 7.45 (d, 1H) ppm.
WORKUP
后处理
- extractionfollowed by extraction with AcOEt
- washThe combined organics are washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated