反应详情

To a solution of 2,4-dichloro-5,7-dihydrothieno[3,4-d]pyrimidine (300 mg, 1.45 mmol) and Et3N (294 mg, 2.9 mmol) in DMF (5.0 mL) at 0° C. was added 3-(S)-methylmorpholine (161 mg, 1.59 mmol) dropwise. After the addition was complete, the mixture was stirred overnight at rt. The solvent was removed under vacuum to give a residue which was partitioned between water and ethyl acetate. The organic layer was washed with brine, dried and concentrated to give the crude product which was purified by preparative TLC (Eluent: petroleum ether/ethyl acetate=2/1) to provide 2-chloro-5,7-dihydro-4-((S)-3-methylmorpholino)thieno[3,4-d]pyrimidine as a light yellow solid (283 mg, 72%).

1. additionAfter the addition
2. customThe solvent was removed under vacuum
3. customto give a residue which
4. customwas partitioned between water and ethyl acetate
5. washThe organic layer was washed with brine
6. customdried
7. concentrationconcentrated
8. customto give the crude product which
9. customwas purified by preparative TLC (Eluent: petroleum ether/ethyl acetate=2/1)