反应详情

温度

90 °C

To a solution of dimethyl 1-(2-azidoethyl)-4-benzyloxy-1H-pyrazole-3,5-dicarboxylate (0.84 g, 2.34 mmol) in anhydrous DMF at 0° C. was added triphenylphosphine (0.92 g, 3.50 mmol). Water (300 μL) was added and the reaction was heated to 90° C. for 3 days. The solvent was removed in vacuo, and the resulting white solid was purified by flash chromatography on silica gel using 0-10% MeOH/CHCl3 gradient elution. Collection and concentration of the appropriate fractions afforded an oily solid which was triturated with methanol to yield a white precipitate. The solid was collected by vacuum filtration to afford the title product. ES MS (M+1)=302.

1. customThe solvent was removed in vacuo
2. customthe resulting white solid was purified by flash chromatography on silica gel using 0-10% MeOH/CHCl3 gradient elution
3. customCollection and concentration of the appropriate fractions
4. customafforded an oily solid which
5. customwas triturated with methanol
6. customto yield a white precipitate
7. filtrationThe solid was collected by vacuum filtration