HRID390401

反应详情

EQUATION

反应方程式

HRID 390401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1′-[4-(bromomethyl)benzyl]-2,3-dihydrospiro[indene-1,4′-piperidine] (0.35 g, 0.94 mmol), ethyl 3-(2-fluoro-4-hydroxyphenyl)propanoate (0.2 g, 0.94 mmol) and K2CO3 (0.32 g, 2.3 mmol) in DMF (15 mL) is stirred overnight at room temperature. The reaction mixture is diluted with cold water and extracted with DCM (3×50 mL). The combined organic layer is washed with brine solution, dried over Na2SO4, and concentrated under vacuum. The crude material is purified by silica gel chromatography (gradient DCM/MeOH 8/2) to give the title compound as an off-white solid (0.22 g, crude). ESI/MS 502 (M+H)+.

WORKUP

后处理

  1. extractionextracted with DCM (3×50 mL)
  2. washThe combined organic layer is washed with brine solution
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under vacuum
  5. customThe crude material is purified by silica gel chromatography (gradient DCM/MeOH 8/2)