反应详情

温度

100 °C

To butan-1-ol (76 mL) was added portion wise sodium tert-butoxide (15.2 g) (Note: reaction mixture gets warm). The above was stirred until homogeneous (ca. 15 min) before 2-chloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (10.0 g) was then added to the resultant pale yellow solution. The reaction mixture was then heated to 100° C., overnight. The reaction mixture was stripped to remove as much butan-1-ol as possible before being partitioned between diethyl ether and water. The diethyl ether phase was separated and the aqueous re-extracted further with diethyl ether. Combined organic layers dried over magnesium sulphate (anhydrous). Magnesium sulphate was filtered off and filtrate stripped to give brown viscous oil which was azeotroped with toluene (3 times) and placed under high vacuum overnight, transferred to new flask with dichloromethane and stripped, placed under high vacuum to give the title compound as a brown glass (9.45 g).

1. additionwas then added to the resultant pale yellow solution
2. customto remove as much butan-1-ol as possible
3. custombefore being partitioned between diethyl ether and water
4. customThe diethyl ether phase was separated
5. extractionthe aqueous re-extracted further with diethyl ether
6. dry with materialCombined organic layers dried over magnesium sulphate (anhydrous)
7. filtrationMagnesium sulphate was filtered off
8. customto give brown viscous oil which
9. customwas azeotroped with toluene (3 times)
10. customplaced under high vacuum overnight
11. customtransferred to new flask with dichloromethane