HRID1283626

反应详情

EQUATION

反应方程式

HRID 1283626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 9 g. (0.028 mole) of 7-(4-chlorobenzoyl)-3-methylthioindolin-2-one in 180 ml. of tetrahydrofuran was treated over a two-hour period with 45 g. of a commercial Raney nickel water suspension. After the addition was complete the mixture was filtered. A drop of concentrated hydrochloric acid was added to the filtrate which removed some color and the resulting solution was then stripped under water pump vacuum to yield a cream color material. Recrystallization from toluene gave pink needles, (93% yield); the material sintered at 177°C. and melted at 186°C.

WORKUP

后处理

  1. additionAfter the addition
  2. filtrationwas filtered
  3. additionA drop of concentrated hydrochloric acid was added to the filtrate which
  4. customremoved some color
  5. customto yield a cream color material
  6. customRecrystallization from toluene
  7. customgave pink needles, (93% yield)
  8. customsintered at 177°C.