HRID2291557

反应详情

EQUATION

反应方程式

HRID 2291557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,4-Dichloronitrobenzene (10 g), piperazine (30 g) and dioxan (10 ml) were stirred for 4 hours under gentle reflux (internal temp. 120°-130°). The mixture was then cooled and water (50 ml) was added; the desired product crystallized out and was filtered off, washed with water and dried: yield of the compound 11.32 g. A small portion (0.6 g) was recrystallized from petroleum b.p. 60°-80°/ethyl acetate, yielding the product, (0.36 g), m.p. 100°-102°.

WORKUP

后处理

  1. temperatureunder gentle reflux (internal temp. 120°-130°)
  2. temperatureThe mixture was then cooled
  3. customthe desired product crystallized out and
  4. filtrationwas filtered off
  5. washwashed with water
  6. customdried
  7. customA small portion (0.6 g) was recrystallized from petroleum b.p. 60°-80°/ethyl acetate
  8. customyielding the product, (0.36 g), m.p. 100°-102°