反应详情

DIPEA (297 mg, 2.3 mmol), HOBT (128 mg, 0.95 mmol), 2-chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid (Method 9, 154 mg., 0.767 mmol) and 3-amino-3,4-dihydro-1,7-naphthyridin-2(1H)-one (Method 28, 300 mg, 0.767 mmol) were suspended in DCM (10 mL). EDCI (183 mg, 0.95 mmol) was then added and the reaction mixture stirred at ambient temperature for 2 hrs. The reaction mixture was filtered and the filtrate was diluted with ethyl acetate (100 mL), washed with saturated aqueous sodium bicarbonate (2×25 mL) and brine (25 mL), dried (MgSO4) and evaporated under reduced pressure to give a light brown solid which was washed with methanol (20 mL) and dried to give the title compound (45 mg, 17%).

1. filtrationThe reaction mixture was filtered
2. additionthe filtrate was diluted with ethyl acetate (100 mL)
3. washwashed with saturated aqueous sodium bicarbonate (2×25 mL) and brine (25 mL)
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure
6. customto give a light brown solid which
7. washwas washed with methanol (20 mL)
8. customdried