HRID1470485

反应详情

EQUATION

反应方程式

HRID 1470485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred solution of 1,5-dihydroxy naphthalene (40 g, 0.25 mol) in dry acetone (200 mL) was added, K2CO3 (34.5 g, 0.25 mol) and the mixture was stirred at RT for 3 h, and then cooled to 0° C. To this, a solution of methyl iodide (124.5 mL, 2 mol) in dry acetone (100 mL) was added drop wise and the reaction mixture was stirred for 2 h at 0° C. and then for 10 h at RT. After completion (TLC), the mixture was filtered and washed with EtOAc. The solvent was removed under reduced pressure and the crude product was purified by column chromatography (8% EtOAc:Hexanes) to afford the desired compound (19.2 g, 44%) as a light green solid.

WORKUP

后处理

  1. waitfor 10 h at RT
  2. filtrationAfter completion (TLC), the mixture was filtered
  3. washwashed with EtOAc
  4. customThe solvent was removed under reduced pressure
  5. customthe crude product was purified by column chromatography (8% EtOAc:Hexanes)