反应详情

To a stirred solution of 3-methoxy-4-[3-(5-methyl-pyrazin-2-yl)ureido]-benzoic acid (30 mg, 0.1 mmol) in 1 mL NMP at RT in a capped reaction vial was added HBTU (42 mg, 0.11 mmol). The suspension was stirred for 15 minutes and then treated with 2-ethylaminopyridine (13.2 μL, 0.11 mmol) followed by Hunigs Base (35 μL, 0.2 mmol). After stirring overnight, NMP was removed by bulb to bulb transfer at 70° C. under high vacuum and the residue stirred with a mixture of CH2Cl2 (10 mL) and 10% Na2CO3 (10 mL) until complete dissolution occurred. The organics were isolated, dried (MgSO4), filtered and concentrated. The residue was triturated with EtOAc to produce a solid which was isolated by filtration (71% yield).

1. stirringAfter stirring overnight
2. customNMP was removed by bulb to bulb transfer at 70° C. under high vacuum
3. stirringthe residue stirred with a mixture of CH2Cl2 (10 mL) and 10% Na2CO3 (10 mL) until complete dissolution
4. customThe organics were isolated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was triturated with EtOAc
9. customto produce a solid which
10. customwas isolated by filtration (71% yield)