HRID1634524

反应详情

EQUATION

反应方程式

HRID 1634524 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzyl 5-acetoxymethyl-2-methoxybenzoate (630 mg, 2.00 mmol), methyl trimethylsilyldimethylketeneacetal (730 mg, 4.02 mmol) and 25 ml of dehydrated methylene chloride were mixed and magnesium perchlorate (45 mg, 0.202 mmol) was added under an atmosphere of argon, which was stirred for 6 hours at room temperature. The reaction mixture was washed with water and with brine, then dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=8:1 v/v) to obtain 131 mg (18%) of the title compound as colorless crystals.

WORKUP

后处理

  1. washThe reaction mixture was washed with water and with brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=8:1 v/v)