反应详情

温度

60 °C

3-Bromopropan-1-ol (0.645 ml, 7.14 mmol) was added to a suspension of (1,3-Dimethyl-2,4-dioxo-5-phenyl-1,2,3,4-tetrahydro-pyrrolo[3,4-d]pyrimidin-6-yl)-carbamic acid benzyl ester (step 1) (2.22 g, 5.49 mmol), K2CO3 (2.276 g, 16.47 mmol) and benzyltrimethylammonium chloride (0.102 g, 0.549 mmol) in acetonitrile (50 ml). The mixture was heated to 60° C. and stirred for 40 mins. The reaction mixture was cooled to RT and diluted with water. The mixture was extracted with EtOAc (2×) and the combined organic phases washed with brine, dried over sodium sulphate and evaporated under reduced pressure. Purification by chromatography on silica, eluting with EtOAc/hexane and then MeOH/EtOAc afforded the title compound as a white foam.

1. temperatureThe reaction mixture was cooled to RT
2. extractionThe mixture was extracted with EtOAc (2×)
3. washthe combined organic phases washed with brine
4. dry with materialdried over sodium sulphate
5. customevaporated under reduced pressure
6. customPurification by chromatography on silica
7. washeluting with EtOAc/hexane