反应详情

温度

10 °C

4-Chloro-2,6-dimethyl-5H-pyrrolo[3,2-d]pyrimidine from example A7 (10.90 g; 60.00 mmol) is dissolved in dichloromethane (120 mL). The stirred mixture is cooled to 10° C. Br2 (3.08 mL; 60.00 mmol) dissolved in dichloromethane (20 mL) is added dropwise within 25 minutes. The resulting precipitate is collected by suction filtration, suspended in Na2SO3 (5% solution) (100 mL) and is stirred for 30 minutes at ambient temperature. After filtratrion the product is dissolved in acetonitrile (1000 mL), refluxed for one hour and filtered while still hot. The solvent is removed under reduced pressure until the product starts to precipitate. Precipitation of the product is completed by addition of cyclohexane and cooling to 0° C. for several hours. The solid is collected by suction filtration, washed with cyclohexane and dried in vacuum at 50° C. over night to yield the title compound as a white solid.

1. additionis added dropwise within 25 minutes
2. filtrationThe resulting precipitate is collected by suction filtration
3. dissolutionis dissolved in acetonitrile (1000 mL)
4. temperaturerefluxed for one hour
5. filtrationfiltered while still hot
6. customThe solvent is removed under reduced pressure until the product
7. customto precipitate
8. customPrecipitation of the product
9. additionis completed by addition of cyclohexane
10. temperaturecooling to 0° C. for several hours
11. filtrationThe solid is collected by suction filtration
12. washwashed with cyclohexane
13. customdried in vacuum at 50° C. over night