HRID973466
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
According to the method of Chem. Abs., 1962, 57, 9840a, a solution of sodium dithionite (85%, 24.74 g, 121 mmol) in water (120 ml) was added to a suspension of (4-iodophenyl)-2-nitroaniline in ethanol (500 ml). The mixture was heated under reflux for 45 minutes, cooled, treated with 300 ml of dilute aqueous ammonia, and concentrated under reduced pressure. The resulting white slurry was treated with 200 ml of dilute aqueous ammonia, filtered and washed with water (200 ml). The solid was dried in a vacuum desiccator at room temperature to give N-(4-iodophenyl)1,2-diaminobenzene, 8.91 g, which gradually darkens on exposure to light, m.p. 122°-123° C.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 45 minutes
- temperaturecooled
- concentrationconcentrated under reduced pressure
- additionThe resulting white slurry was treated with 200 ml of dilute aqueous ammonia
- filtrationfiltered
- washwashed with water (200 ml)
- customThe solid was dried in a vacuum desiccator at room temperature