HRID4930

反应详情

EQUATION

反应方程式

HRID 4930 的结构方程式

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

Into concentrated hydrochloric acid (63.6 ml) was dissolved N-acetyl-7-cyano-5-nitroindoline (5.3 g), which was then subjected to stirring at 140° C. for 45 minutes. The reaction mixture was cooled to 0° C. to give deposited crystal, which was then collected by filtration. The obtained crude crystal was suspended into water (50 ml), and was rendered basic by adding 50% sodium hydroxide, and the insoluble matter was collected by filtration. After adding concentrated hydrochloric acid to the filtrate, the deposited crystal was collected by filtration and dried to give the intended compound 3.7 g (77.1%) as yellow powder. M.P.: 294°-297° C. (decomp.)

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customto give
  3. filtrationwas then collected by filtration
  4. customThe obtained crude crystal
  5. filtrationthe insoluble matter was collected by filtration
  6. additionAfter adding concentrated hydrochloric acid to the filtrate
  7. filtrationthe deposited crystal was collected by filtration
  8. customdried