HRID1902593

反应详情

EQUATION

反应方程式

HRID 1902593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

68.3 gm of 2-chloro-4-nitro-1,3-diphenoxy-benzene were dissolved in 300 ml of toluene, and the solution was admixed with 100 ml of concentrated aqueous ammonia in an autoclave. The autoclave was then closed, the internal pressure was increased to 3 bar with gaseous ammonia, and the contents were heated for 12 hours at 120° C., whereby the internal pressure rose to about 13 bar. Thereafter, the contents were allowed to cool, and the organic phase was separated, extracted with dilute hydrochloric acid, dried with sodium sulfate and the toluene was distilled off. The reaction product was obtained with virtually quantitative yield (54 gm). Gas-chromatographic analysis revealed that the reaction product contained 98% of the title compound, m.p. 81°-82° C.

WORKUP

后处理

  1. customThe autoclave was then closed
  2. temperatureto cool
  3. customthe organic phase was separated
  4. extractionextracted with dilute hydrochloric acid
  5. dry with materialdried with sodium sulfate
  6. distillationthe toluene was distilled off
  7. customThe reaction product was obtained with virtually quantitative yield (54 gm)