反应详情

温度

-5 °C

A solution of 4.0 g (0.012 mole) of 3-(4-bromophenacyl)-2,3,5,6-tetrahydrothiopyran-4-one [Example 2 (a)], 1.3 g of ethylaminoethylamine, 14 ml. of ethanol, and one drop of concentrated hydrochloric acid is heated under reflux for 2.5 hours, cooled to -5°C, and diluted with water. The oil which separates is collected and triturated with water to provide a solid. The resultant solid is recrystallized from ethanol to give off-white crystals of 1-(2-ethylaminoethyl)-2-(4-bromophenyl)-1,4,6,7-tetrahydrothiopyrano[4,3-b]pyrrole, m.p. 84° to 85°C.

1. temperatureunder reflux for 2.5 hours
2. customThe oil which separates is collected
3. customtriturated with water
4. customto provide a solid
5. customThe resultant solid is recrystallized from ethanol