反应详情

Into 75 mL of acetone was successively added [4.2 g, 10.65 mmol] of 2-Bromo-1-[7-(toluene-4-sulfonyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-ethanone followed by [0.81 g, 10.65 mmol] of thiourea. The reaction was then stirred for 4.0 hours at ambient temperature. The pale yellow precipitate was collected via suction filtration and washed with more acetone. The crude cake was suspended into 20 mL of triethylamine and stirred for one hour. The material was then diluted with water and suction filtered to isolate the solid. The damp cake was triturated with acetonitrile, the solid isolated again via suction filtration and airdried. The beige solid, 2.6 g, represents a 72% yield of the free base.

1. filtrationThe pale yellow precipitate was collected via suction filtration
2. washwashed with more acetone
3. stirringstirred for one hour
4. additionThe material was then diluted with water and suction
5. filtrationfiltered
6. customto isolate the solid
7. customThe damp cake was triturated with acetonitrile
8. customthe solid isolated again via suction filtration