HRID1874845
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-{[3-(bromomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile (1.04 g, 2.77 mmol) in CH2Cl2 (10 mL) was added dropwise to a 2M solution of MeNH2 (13.9 mL, 27.73 mmol) in THF. The solution turned light yellow and the flask was stoppered and stirred at RT overnight. Ethyl acetate (200 ml) and saturated NaHCO3 solution (150 ml) were added. The organic layer was separated, washed with brine (150 mL), dried over MgSO4, filtered and concentrated to give the title compound (0.81 g, 90%) as a yellow oil. 1H NMR (400 MHz, CDCl3) δ ppm 7.30-7.33 (m, 1H), 7.24-7.30 (m, 2H), 7.11-7.14 (m, 1H), 6.98 (dd, 1H), 3.81 (s, 2H), 2.45 (s, 3H).
WORKUP
后处理
- customThe organic layer was separated
- washwashed with brine (150 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated