反应详情

温度

45 °C

9.8 g (0.2 mol) of sodium cyanide is dissolved in 70 ml of water and to the solution first 32.8 g (0.2 mol) of 2-(2-thienyl)ethylamine hydrochloride, then in a period of a few minutes, the solution of 28.2 g (0.2 mol) of o-chlorobenzaldehyde in 30 ml of ethanol are added. During the addition the temperature of the mixture raises to 45° C. The reaction mixture is then stirred at 60° C. for 2 hours, then cooled to room temperature and diluted with 50 ml of water. The resulting oily product is extracted with 100 ml of 1,2-dichloroethane, the organic phase is washed to cyanide-free with 2×50 ml of water, the traces of 2-(2-thienyl)ethylamine are removed by treatment with 20 ml of 3% hydrochloric acid solution. The residual fast crystallizing oil is the product. Weight: 52 g (94%) mp.: 40-41° C. The product was identified as written in Example 1. Quality of the product is identical with that of the product prepared according to Example 1.

1. waitin a period of a few minutes
2. additionDuring the addition the temperature of the mixture
3. temperaturecooled to room temperature
4. extractionThe resulting oily product is extracted with 100 ml of 1,2-dichloroethane
5. washthe organic phase is washed to cyanide-free with 2×50 ml of water
6. customthe traces of 2-(2-thienyl)ethylamine are removed by treatment with 20 ml of 3% hydrochloric acid solution
7. customThe residual fast crystallizing oil
8. customprepared