HRID1374770

反应详情

EQUATION

反应方程式

HRID 1374770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 7-iodo-6-methyl-1H-quinolin-4-one (5.12 g, 18.0 mmol), phosphorus oxide chloride (14 mL) and N,N-dimethylformamide (1 mL) was stirred at 60° C. for 80 min, then poured onto ice and carefully neutralized with 25% aq. ammonium hydroxide solution. The suspension was extracted three times with dichloromethane, the combined organic phase was washed with brine, dried (MgSO4), and evaporated to afford the title compound (5.33 g, 98%). Light brown solid, ISP-MS: m/e=304.1 ([M+H]+).

WORKUP

后处理

  1. additionpoured onto ice
  2. extractionThe suspension was extracted three times with dichloromethane
  3. washthe combined organic phase was washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated