HRID2063830

反应详情

EQUATION

反应方程式

HRID 2063830 的结构方程式

PROCEDURE

实验过程

A solution of N,N-diethylaniline (12.1 mL) containing 1-chloro-2-methyl-3-[(2-methylprop-2-en-1-yl)oxy]benzene (3.00 mg, 15.3 mmol) synthesized in Reference Example 153 was reacted under microwave irradiation at 220° C. for 20 minutes. After cooled to room temperature, the reaction solution was diluted with ethyl acetate, and washed serially with 1N hydrochloric acid, saturated sodium bicarbonate water and saturated saline. It was dried using anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. After that, the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 10:1) to give 2.89 g of the title compound as a yellow solid (yield: 96%).

WORKUP

后处理

  1. customsynthesized in Reference Example 153
  2. customwas reacted under microwave irradiation at 220° C. for 20 minutes
  3. washwashed serially with 1N hydrochloric acid, saturated sodium bicarbonate water and saturated saline
  4. customIt was dried
  5. customthe solvent was removed under reduced pressure
  6. customAfter that, the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 10:1)