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
10.7 g (40 mmol) of 3-acetamido-2-phenyl-benzo(b)thiophene and 3.8 g (0.1 mol) of LiAlH4 in 200 milliliters of absolute dioxan is refluxed with stirring for 1 hour. The cooled reaction mixture is mixed with water to decompose the excess LiAlH4 and, after the addition of 300 milliliters of CH2Cl2, it is stirred for a further 15 minutes. After centrifuging with the addition of hyflo, the organic phase is dried over potassium carbonate and evaporated: 3-ethylamino-2-phenyl-benzo(b)thiophene in the form of a crude oily product. It is dissolved in a little chloroform and converted into the hydrochloride by hydrochloric gas: 10.9 g (94% of theory) of colourless sticks in ethanol, decomposition from 205° C. (in sealed tube).
WORKUP
后处理
- customThe cooled reaction mixture
- stirringis stirred for a further 15 minutes
- additionAfter centrifuging with the addition of hyflo
- dry with materialthe organic phase is dried over potassium carbonate
- customevaporated
- dissolutionIt is dissolved in a little chloroform
- customfrom 205° C.