反应详情

To a solution of (5-chloro-7-morpholinothiazolo[4,5-d]pyrimidin-2-yl)methanol 56 (100 mg, 0.4 mmol) in benzene (3.0 mL) at 0° C. was added PBr3(30 μL, 0.4 mmol). The reaction was heated at reflux for 1 hour. After cooling to room temperature the reaction was quenched by the addition of water. The aqueous layer was extracted with EtOAc. The combined organics were dried over Na2SO4 and concentrated in vacuo. The crude 4-(2-(bromomethyl)-5-chlorothiazolo[4,5-d]pyrimidin-7-yl)morpholine 57 did not require further purification (x mg, x %). MS (Q1)×(M)+

1. temperatureThe reaction was heated
2. temperatureat reflux for 1 hour
3. customwas quenched by the addition of water
4. extractionThe aqueous layer was extracted with EtOAc
5. dry with materialThe combined organics were dried over Na2SO4
6. concentrationconcentrated in vacuo
7. custompurification (x mg, x %)