HRID1464821

反应详情

EQUATION

反应方程式

HRID 1464821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(R)-(-)-3,4-Dihydro-2-(4-hydroxybenzyl)-2H-benzopyran (5.0 g, 20 mmol), 4-dimethylaminopyridine (240 mg, 2 mmol), triethylamine (2.6 g, 25 mmol) and acetic anhydride (2.9 g, 28 mmol) were dissolved in methylene chloride (75 ml) and stirred at room temperature for 2 hours under a nitrogen atmosphere. The solvent was removed in vacuo and the residue purified on silica gel using hexanes/ethyl acetate (3:1) as eluent to afford an oil which was crystallized from hexanes to yield 4.0 g of the title product, m.p. 64°-65° C.; [α]D -98.9° (c 1.3, MeOH);

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe residue purified on silica gel
  3. customto afford an oil which
  4. customwas crystallized from hexanes