反应详情

3.0 g (11.8 mmol) of 3-formamido-2-phenyl-benzo(b)thiophene and 1.08 g (28.4 mmol) of lithium hydride and aluminium are refluxed with stirring for 30 minutes in 60 milliliters of absolute dioxane. The cooled reaction mixture is mixed with water to decompose the excess lithium and aluminium hydride and, after the addition of approximately 100 milliliters of CH2Cl2, it is stirred for a further 15 minutes. After centrifuging with the addition of the hyflo, the organic phase is dried over K2CO3 and evaporated: 3-methylamino-2-phenyl-benzo(b)thiophene in the form of a crude oily product. It is dissolved in a little CHCl3 and converted into the hydrochloride by hydrochloric gas: 2.6 g (80% of theory) of colourless crystals in a mixture of ethanol and ether, decomposition from 198° C. (in sealed tubes).

1. customThe cooled reaction mixture
2. additionAfter centrifuging with the addition of the hyflo
3. dry with materialthe organic phase is dried over K2CO3
4. customevaporated
5. dissolutionIt is dissolved in a little CHCl3
6. addition2.6 g (80% of theory) of colourless crystals in a mixture of ethanol and ether, decomposition from 198° C. (in sealed tubes)