反应详情

To a solution of 6.32 g (13 mmol) of the compound of Example 1 in 150 mL of toluene at ambient temperature is added dropwise a solution of 0.24 mL (13 mmol) of distilled water in 3.0 mL (22 mmol) of triethylamine. After the addition is complete, the reaction mixture is stirred at ambient temperature for 15 minutes. The reaction solvent is removed in vacue and the reaction mass is then recrystallized twice with 50 mL of acetonitrile. The recrystallization solvent is removed under vacuum and the residue is dried under vacuum to afford the title compound in a yield of 5.2 g (86.3%) as an off-white solid melting at 218° C.

1. additionAfter the addition
2. customThe reaction solvent is removed in vacue
3. customthe reaction mass is then recrystallized twice with 50 mL of acetonitrile
4. customThe recrystallization solvent is removed under vacuum
5. customthe residue is dried under vacuum