反应详情

To a solution of 2,4-dichloro-5,7-dihydrothieno[3,4-d]pyrimidine 6,6-dioxide (120 mg, 0.5 mmol) and Et3N (101 mg, 1.0 mmol) in DMF (5.0 mL) at 0° C. was added a mixture of(S)-3-methylmorpholine (51 mg, 0.5 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 (Na2SO4) and concentrated to give the 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 6,6-dioxide as a light yellow solid (100 mg, 66%).

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. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customto give the product which
9. customwas purified by preparative TLC (Eluent: petroleum ether/ethyl acetate=2/1)