HRID503990

反应详情

EQUATION

反应方程式

HRID 503990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

5-Trifluoromethanesulfonyloxy-3,4-dihydro-1H-quinolin-2-one (1.5 g), zinc cyanide (1.3 g) and tetrakis(triphenylphosphine)palladium (0.59 g) were suspended in DMF (20 ml), and the suspension was stirred at 100° C. for 2 hours. The insoluble matter was filtered off, and ethyl acetate was added to the filtrate, followed by washing with water. The resulting mixture was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure, and the residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent to thereby obtain 0.71 g (yield: 81%) of 5-cyano-3,4-dihydro-1H-quinolin-2-one as a light brown powder.

WORKUP

后处理

  1. filtrationThe insoluble matter was filtered off
  2. additionethyl acetate was added to the filtrate
  3. washby washing with water
  4. dry with materialThe resulting mixture was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customthe residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent