HRID1850395

反应详情

EQUATION

反应方程式

HRID 1850395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium carbonate (1.23 g, 8.92 mmol) and chloromethylmethylether (539 mg, 6.69 mmol) were sequentially added to a suspension of DMF (20 mL) containing 7-hydroxy-2,2,4,6-tetramethyl-1-benzofuran-3(2H)-one (920 mg, 4.46 mmol) synthesized in Reference Example 69 at 0° C. The reaction solution was warmed to room temperature and stirred for 15 hours. The resulting mixture was poured into saturated sodium bicarbonate water, and extraction was performed using ethyl acetate. The extract was washed with saturated saline, and dried using anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was purified by silica gel chromatography (hexane-ethyl acetate 95:5 to 85/15) to give 920 mg of the title compound (yield: 82%).

WORKUP

后处理

  1. customsynthesized in Reference Example 69 at 0° C
  2. washThe extract was washed with saturated saline
  3. customdried
  4. concentrationfollowed by concentration under reduced pressure
  5. customThe residue was purified by silica gel chromatography (hexane-ethyl acetate 95:5 to 85/15)