HRID11491

反应详情

EQUATION

反应方程式

HRID 11491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of 3-[(4-hydroxy-phenylamino)-methylene]-1,3-dihydro-indol-2-one (0.945 g, 3.75 mmol) in 20 mL DMF is treated with potassium carbonate (777 mg, 1.5 equiv.) and 1-bromo-3-chloropropane (1.1 equiv.). The reaction mixture is heated to 40° C. for 3 h. The reaction mixture is partitioned between EtOAc and water. The organic layer is collected and washed sequentially with H2O (1×), saturated aqueous NaHCO3 solution (1×), and brine (1×). The organic phase was dried and concentrated to give an oil. The oil was purified by preparative chromatography (silica gel; 1:1 EtOAc:hexane) to give the named compound as a yellow solid (711 mg, 58%).

WORKUP

后处理

  1. customThe reaction mixture is partitioned between EtOAc and water
  2. customThe organic layer is collected
  3. washwashed sequentially with H2O (1×), saturated aqueous NaHCO3 solution (1×), and brine (1×)
  4. customThe organic phase was dried
  5. concentrationconcentrated
  6. customto give an oil
  7. customThe oil was purified by preparative chromatography (silica gel; 1:1 EtOAc:hexane)