反应详情

6-(3,4-Difluorophenyl)-1,6-dihydro-2-methoxy-5-methoxycarbonyl-4-methyl-1-[(4-nitrophenyloxy)carbonyl]pyrimidine (1.5 mmol, 0.66 g) in 5 mL of chloroform was added a solution of bromine (1.5 mmol, 0.09 mL) in 3 mL of chloroform at 0° C. and the solution was allowed to attain room temperature over 1.5 h. The solvent was removed in vacuo and the residue was again dissolved in CHCl3 (20 mL) and washed with brine. The organic layer was separated, dried over Na2SO4, filtered and the solvent was removed in vacuo to afford the desired product as a yellow foam, which was used in the next step without purification. 1H NMR δ 3.75 (s, 3 H), 4.67 (ABq, 2 H), 6.35 (s, 1 H), 7.09-7.19 (m, 4 H), 7.37 (d, J=9.0 Hz, 2 H), 8.27 (d, J=9.0 Hz, 2 H).

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was again dissolved in CHCl3 (20 mL)
3. washwashed with brine
4. customThe organic layer was separated
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customthe solvent was removed in vacuo