HRID1464699
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
8-Bromo-3-nitrochroman (400 mg; 1.55 mmol) was dissolved in glacial acetic acid (30 ml) and zinc dust (2 g) was added. The mixture was heated to 100° C. for 15 minutes. The zinc dust was filtered off and washed with dichloromethane. The solvent was evaporated and the remaining oil extracted with diluted hydrochloric acid/dichloromethane. The phases were separated and the pH of the water layer was adjusted to 11 with 2N NaOH. The water layer was extracted with dichloro-methane. The phases were separated and the organic layer dried (Na2SO4). The solvent was evaporated yielding 214 mg (61%) of 8-bromo-3-aminochroman.
WORKUP
后处理
- filtrationThe zinc dust was filtered off
- washwashed with dichloromethane
- customThe solvent was evaporated
- extractionthe remaining oil extracted with diluted hydrochloric acid/dichloromethane
- customThe phases were separated
- extractionThe water layer was extracted with dichloro-methane
- customThe phases were separated
- dry with materialthe organic layer dried (Na2SO4)
- customThe solvent was evaporated