HRID440128
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
- 70 °C
PROCEDURE
实验过程
A mixture of 4-benzyl-2-nitrophenol (1.3 g, 5.3 mmol) and K2CO3 (1.2 g, 8.7 mmol) in DMF (10 mL) was stirred for 10 min. Dibromoethane (1.4 mL, 16.2 mmol) was added to the reaction mixture and heated at 70° C. for 24 hrs. The reaction mixture was diluted with ether (30 mL) and washed with water (20 mL) and brine (20 mL). The ether layer was dried (MgSO4) and concentrated under reduced pressure. The crude product was fractionated by flash chromatography (4:1 hexane/ethyl acetate) yielding bromoethane 6 as a yellow oil (1.3 g, 88%). 1H NMR: 3.65 (t, J=5 Hz, 2H), 4.35 (t, J=5 Hz, 2H), 5.05 (s, 2H), 7.0-7.5 (m, 8H).
WORKUP
后处理
- washwashed with water (20 mL) and brine (20 mL)
- dry with materialThe ether layer was dried (MgSO4)
- concentrationconcentrated under reduced pressure