HRID1597220

反应详情

EQUATION

反应方程式

HRID 1597220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

1-(2-Chloroethyl)pyrrolidine hydrochloride (1.27 g, 7.5 mmol) was added to 7-hydroxy-6-methoxy-4-phenoxyquinazoline (1.0 g, 3.7 mmol), and potassium carbonate (3.9 g, 28.3 mmol) in DMF (30 ml). The mixture was heated at 110° C. for 4 hours and allowed to cool. The mixture was filtered, and the volatiles were removed from the filtrate by evaporation. The residue was purified by column chromatography eluting with methylene chloride/methanol/ammonia, (100/8/1) to give an oil which was triturated with ethyl acetate to give 6-methoxy-4-phenoxy-7-(2-(pyrrolidin-1-yl)ethoxy)quinazoline (200 mg, 15%) as a white solid.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationThe mixture was filtered
  3. customthe volatiles were removed from the filtrate by evaporation
  4. customThe residue was purified by column chromatography
  5. washeluting with methylene chloride/methanol/ammonia, (100/8/1)
  6. customto give an oil which
  7. customwas triturated with ethyl acetate