HRID65931

反应详情

EQUATION

反应方程式

HRID 65931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

114 Grams (2.01 moles) of iron powder are added to a solution of 134 g (0.64 mole) of 5-chloro-6-nitro-1-indanone in 1600 ml of ethanol, then 63.5 ml of concentrated hydrochloric acid are added dropwise, and the reaction mixture is boiled for 4 hours. The precipitate is filtered off with suction, and the product is precipitated from the hot filtrate by the addition of water, then suction-filtered and washed with water. The residue of the reaction mixture is boiled with chloroform, the filtrate is dried with Na2SO4 and is then concentrated to dryness, after which process a further amount of the product is obtained. The substance melts at a temperature of from 198° to 200° C., and after recyrstallization from ethanol the melting point is in the range of from 203° to 205° C.

WORKUP

后处理

  1. filtrationThe precipitate is filtered off with suction
  2. customthe product is precipitated from the hot filtrate by the addition of water
  3. filtrationsuction-filtered
  4. washwashed with water
  5. dry with materialthe filtrate is dried with Na2SO4
  6. concentrationis then concentrated to dryness
  7. customafter which process a further amount of the product is obtained
  8. custommelts at a temperature of from 198° to 200° C.
  9. customis in the range of from 203° to 205° C.