反应详情

8.0 g (36 mmol) of the compound from Step 9.1 was dissolved in 50 mL of acetonitrile and to the solution was added dropwise 4.55 g (36 mmol) of dimethyl sulfate over a period of 5 minutes with agitation which caused the reaction mixture to warm up slightly while the product gradually separated in crystalline form. The mixture was allowed to agitate for an additional 3 hours at room temperature after which it was suction-filtered. The filter cake was washed with a small amount of acetonitrile and then dried at 40° C. under vacuum. This gave 11.0 g (88% of the theoretical) of yellow crystals.

1. temperatureto warm up slightly while the product
2. customgradually separated in crystalline form
3. filtrationwas suction-filtered
4. washThe filter cake was washed with a small amount of acetonitrile
5. customdried at 40° C. under vacuum