反应详情

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