反应详情

To a mixture of 4-(2-amino-2-oxoethyl)-N-(4-chlorobenzyl)-2-(hydroxymethyl)-3-methyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (58 mg, 0.13 mmol), collidine (44 μL, 0.33 mmol) and DMAP (2.4 mg) in DMF (2.25 mL) was added methanesulfonyl chloride (26 μL, 0.33 mmol). The mixture was stirred at room temperature for 48 hrs. Additional reagents (half original amounts) were added and the reaction was stirred another 4 hrs. The reaction was chilled in ice before the addition of water (8 mL). The ppt was collected by filtration, washed with water and dried in vacuo, giving the title compound as a white solid (58 mg).

1. additionAdditional reagents (half original amounts) were added
2. stirringthe reaction was stirred another 4 hrs
3. filtrationThe ppt was collected by filtration
4. washwashed with water
5. customdried in vacuo