反应详情

温度

-40 °C

Following the procedures in U.S. Pat. No. 6,492,383, 2.5 M of n-butyllithium (9.4 mL, 22.48 mmol) in hexane solution was added to a mixture of 4-(5-chlorothiazolo[4,5-d]pyrimidin-7-yl)morpholine 16 (3.0 g, 11.74 mmol) in 60 mL of THF at −78° C. The reaction mixture was allowed to warm to −40° C. and stirred for 30 min. A solution of iodine (6.0 g, 23.48 mmol) in 10 mL of THF was added dropwise. After the addition was completed. The reaction mixture was brought to room temperature and stirred for 2 h. The mixture was quenched by diluting with dichloromethane and extracting with H2O (2×100 mL). The organic layer was washed with Na2S2O3 (2×100 mL), H2O (2×100 mL), dried over MgSO4, filtered and evaporated to afford 4-(5-chloro-2-iodothiazolo[4,5-d]pyrimidin-7-yl)morpholine 27.

1. additionAfter the addition
2. customwas brought to room temperature
3. stirringstirred for 2 h
4. customThe mixture was quenched
5. additionby diluting with dichloromethane
6. extractionextracting with H2O (2×100 mL)
7. washThe organic layer was washed with Na2S2O3 (2×100 mL), H2O (2×100 mL)
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customevaporated