HRID744853

反应详情

EQUATION

反应方程式

HRID 744853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 50 g of 4-methoxy-3-(4-methoxy-2-butenyl)-bromobenzene in 700 ml of tetrahydrofuran is hydrogenated for 2 hours under normal pressure and at room temperature in the presence of 2.5 g of 5% Pt/C. The reaction mixture is filtered. The filtrate is concentrated by evaporation. The evaporation residue obtained from the filtrate is purified by FC (1.6 kg of silica gel, hexane/ethyl acetate=20:1). Distillation under a high vacuum yields the title compound: Rt (hexane/ethyl acetate=10:1)=0.38; HPLC Rt =19.92 minutes; FAB-MS (M+H)+ =273.

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered
  2. concentrationThe filtrate is concentrated by evaporation
  3. customThe evaporation residue obtained from the filtrate
  4. customis purified by FC (1.6 kg of silica gel, hexane/ethyl acetate=20:1)
  5. distillationDistillation under a high vacuum