反应详情

Absolute ethanol (20,000 ml) was charged into a 20 gallon flask and stirred under nitrogen atmosphere; 517.62 g (9.58 moles) of sodium methoxide were added. After stirring for 30 minutes there was complete solution and 2,063 g (9.58 moles) of 11H-imidazo[1,2-c][1,3]benzodiazepine-5(6H)-thione were added. There was complete solution after stirring at room temperature for 1 hour. The solution was then cooled to 1°, and 1,360 g (9.58 moles) of methyl iodide were added over 30 minutes. The reaction mixtue was stirred at 5° for 4 hours and at ambient temperature overnight. The turbid solution was then cooled to 5° and diluted with 50,000 ml of water. The resulting suspension was stirred for 4 hours at 5°. The solid was collected, and dried (5 mm Hg/60°) to give 5-methylthio-11H-imidazo[1,2-c][1,3]benzodiazepine, m.p. 87°-8°.

1. stirringAfter stirring for 30 minutes there
2. additionwere added
3. stirringafter stirring at room temperature for 1 hour
4. temperatureThe solution was then cooled to 1°
5. stirringThe reaction mixtue was stirred at 5° for 4 hours and at ambient temperature overnight
6. temperatureThe turbid solution was then cooled to 5°
7. stirringThe resulting suspension was stirred for 4 hours at 5°
8. customThe solid was collected
9. customdried (5 mm Hg/60°)