反应详情

To a solution of (2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methanol 29 (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 product 30 did not require further purification (115 mg, 94%). MS (Q1) 350 (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 (115 mg, 94%)