HRID2179401
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
- 65 °C
PROCEDURE
实验过程
To a solution of the product of step D (500 mg, 1.66 mmol) in THF (8 mL) was added triphenylphosphine (72 mg, 3.32 mmol) followed by water (3 mL). The reaction mixture was heated to 65° C. for 4 h and concentrated in vacuo. Purification by column chromatography (SiO2, 95:5 dichloromethane/methanol) provided 2-(5-bromo-7-chlorobenzofuran-2-yl)ethanamine (388 mg, 85%) as a colorless liquid: 1H NMR (CDCl3, 400 MHz) δ 7.51 (t, J=2.4 Hz, 1H), 7.36 (t, J=2.4 Hz, 1H), 6.45 (s, 1H), 3.12 (t, J=8.4 Hz, 2H), 2.94 (t, J=8.8 Hz, 2H).
WORKUP
后处理
- concentrationconcentrated in vacuo
- customPurification by column chromatography (SiO2, 95:5 dichloromethane/methanol)