HRID2352304
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
4-Nitrobenzenesulphonyl chloride (10 g) was added portionwise to a stirred solution of 4-methoxyphenethylamine (6.8 g) in pyridine (40 ml) and the resulting solution stirred at room temperature for 30 min. The solution was partitioned between hydrochloric acid (5 N, 400 ml) and ethyl acetate (2×250 ml). The combined extracts were washed with hydrochloric acid (5 N, 100 ml), sodium bicarbonate (8%, 100 ml) dried --MgSO4) and evaporated in vacuo to give an oil. The oil was purified by column chromatography eluted with hexane:ethyl acetate (2:1) to give the title compound as a solid (4.7 g) m.p. 92°-93°.
WORKUP
后处理
- customThe solution was partitioned between hydrochloric acid (5 N, 400 ml) and ethyl acetate (2×250 ml)
- washThe combined extracts were washed with hydrochloric acid (5 N, 100 ml), sodium bicarbonate (8%, 100 ml)
- customdried
- customMgSO4) and evaporated in vacuo
- customto give an oil
- customThe oil was purified by column chromatography
- washeluted with hexane:ethyl acetate (2:1)