反应详情

温度

100 °C

1-(5-benzyloxy-7-bromo-1,3-benzothiazol-2-yl)-3-ethyl-urea (1 g, 2.46 mmol) and tributyl-(1-ethoxy-vinyl)-stannane (1.77 g, 4.92 mmol) were dissolved in DMF (30 mL) and the mixture deoxygenated by bubbling N2 through the solution for 20 min. Pd(PPh3)4, (284 mg, 0.246 mmol) was added and the reaction heated to 100° C. for 4 h under a N2 atmosphere, at the end of which time LCMS indicated clean formation of the vinyl ether. The reaction was concentrated under reduced pressure, diluted with EtOAc, washed with water then brine and the organic layer dried (MgSO4), filtered and the solvent removed in vacuo to give the desired compound.

1. customthe mixture deoxygenated
2. customby bubbling N2 through the solution for 20 min
3. concentrationThe reaction was concentrated under reduced pressure
4. additiondiluted with EtOAc
5. washwashed with water
6. dry with materialbrine and the organic layer dried (MgSO4)
7. filtrationfiltered
8. customthe solvent removed in vacuo