HRID1445888

反应详情

EQUATION

反应方程式

HRID 1445888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of sodium hydride (60% in mineral oil, 0.093 g, 6.45 mmole) in DMF (10 mL), (2-methyl-1H-indol-4-yloxy)-acetic acid benzyl ester (2) (0.845 g, 2.3 mmole) was added. The mixture was stirred at room temperature for 1 h. To the mixture, dibromododecane (0.765 g, 2.3 mmole) was added and the reaction mixture was stirred at room temperature for 18 h. The reaction was diluted with ethyl acetate and washed with water. The organic layer was separated, dried with sodium sulphate and concentrated. The residue was purified by column chromatography (10:1, hexane: EtOAc) to afford intermediate 3. Yield: 0.708 g, 45%.

WORKUP

后处理

  1. additionwas added
  2. stirringthe reaction mixture was stirred at room temperature for 18 h
  3. washwashed with water
  4. customThe organic layer was separated
  5. dry with materialdried with sodium sulphate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography (10:1, hexane: EtOAc)