反应详情

温度

70 °C

To a vial containing 4-chlorobenzo[d][1,3]dioxol-5-amine (28.8 mg, 0.168 mmol, 1 equiv.) in 1 mL THF was added 4M HCl in 1,4-dioxane (0.042 mL, 1 equiv.) followed by phosgene (20% in toluene; 0.360 mL, 0.684 mmol, 4 equiv.). The vial was capped and heated to 70° C. for 1 h, the solvent was removed under, the residue redissolved in toluene and solvent was again removed under vacuum to eliminate any remaining phosgene yielding 4-chloro-5-isocyanatobenzo[d][1,3]dioxole used as such in the next step.

1. customThe vial was capped
2. customthe solvent was removed under, the residue
3. dissolutionredissolved in toluene
4. customsolvent was again removed under vacuum