反应详情

温度

118 °C

4-Amino-2-methyl-10H-thieno-[2,3-b][1,5]benzodiazepine (100 g, 0.38 mol), N-methylpiperazine (250 mL, 2.5 vol) and 2-butanol (200 mL, 2 vol) were charged into a three-necked round bottom flask equipped with a reflux condenser, overhead stirrer, and thermometer. The reaction mixture was heated to reflux at 118° C. under a nitrogen atmosphere and refluxed overnight. The reaction mixture was allowed to cool to below 55° C. whereupon water (300 mL, 3 volumes) was added to precipitate out the solid. It was isolated by Buchner filtration and the light yellow solid was washed twice with 25% aqueous 2-butanol (100 mL) and then once with 2-butanol (100 mL) and dried to provide olanzapine in 84% yield (98.7 g).

1. customequipped with a reflux condenser, overhead stirrer
2. temperatureThe reaction mixture was heated
3. temperaturerefluxed overnight
4. additionwas added
5. customto precipitate out the solid
6. customIt was isolated by Buchner filtration
7. washthe light yellow solid was washed twice with 25% aqueous 2-butanol (100 mL)
8. dry with materialonce with 2-butanol (100 mL) and dried