HRID22159

反应详情

EQUATION

反应方程式

HRID 22159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.2 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-methoxyphthalide (see Example 8) are heated at reflux temperature in a 1:1 mixture of tetrahydrofuran and hydrochloric acid for 3 hours. Concentration is then carried out under reduced pressure and the resulting crystals are filtered off and washed with water to yield pure 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide, m.p. 143°-145° C.; IR (KBr): 1770 cm-1 ; 1H-NMR (CDCl3): 6.60 ppm (s, 1H).

WORKUP

后处理

  1. temperatureat reflux temperature
  2. concentrationConcentration
  3. filtrationthe resulting crystals are filtered off
  4. washwashed with water