HRID1453086
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
- 50 °C
PROCEDURE
实验过程
MeOH (16 mmol, 0.81 ml), TMSCI (20 mmol, 2.13 g) and (4-bromo-2-fluorophenyl) acetonitrile (10 mmol, 2.13 g) were sequentially added to a dry flask under a nitrogen atmosphere at room temperature. The reaction mixture was heated at 50° C. for 4 hours. After being cooled to room temperature, water (20 mmol, 0.36 ml) was added to the mixture, followed by the addition of Na2CO3 (10 mmol, 1.06 g) and CH2Cl2 (10 ml). Drying over MgSO4 and concentrating at low pressure afforded product (0.85 g, 35% yield). 1H NMR (300 MHz, CDCl3) δ: 3.57 (s, 2H), 3.65 (s, 3H), 7.08 (t, J=8.3 Hz, 1H), 7.16-7.21 (m, 2H).
WORKUP
后处理
- temperatureAfter being cooled to room temperature
- dry with materialDrying over MgSO4
- concentrationconcentrating at low pressure