HRID484104

反应详情

EQUATION

反应方程式

HRID 484104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 2.15 g of 6-(methylthio)-benz-[cd]indol-2(1H)-one (Example 2), 0.6 g of 60% sodium hydride in 70 ml of N,N-dimethylformamide is heated at 50° C. for 30 minutes then cooled. A solution of 2.22 g of 1-bromo-4-cyano-butane in 25 ml of N,N-dimethylformamide is added dropwise to the reaction mixture and stirring continued for 3 hours. The reaction mixture is quenched in 400 ml of ice water and extracted with (2×300 ml) of ethyl acetate. The organic layer is dried with magnesium sulfate and evaporated to afford a solid which is stirred with ether, filtered and dried to yield 2.5 g of the desired product as a solid, m.p. 120°-122° C.

WORKUP

后处理

  1. temperaturethen cooled
  2. customThe reaction mixture is quenched in 400 ml of ice water
  3. extractionextracted with (2×300 ml) of ethyl acetate
  4. dry with materialThe organic layer is dried with magnesium sulfate
  5. customevaporated
  6. customto afford a solid which
  7. filtrationfiltered
  8. customdried