HRID2291557
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder gentle reflux (internal temp. 120°-130°)
- temperatureThe mixture was then cooled
- customthe desired product crystallized out and
- filtrationwas filtered off
- washwashed with water
- customdried
- customA small portion (0.6 g) was recrystallized from petroleum b.p. 60°-80°/ethyl acetate
- customyielding the product, (0.36 g), m.p. 100°-102°