反应详情

To a mixture of the product of Example 361C (4.2 g, 9.8 mmol) and pyridine (1.6 g, 1.62 mL, 20 mmol) in dichloromethane (100 mL) was added dropwise 2,2,2-trichloroethyl chloroformate (2.29 g, 10.8 mmol) over 30 minutes. The reaction mixture was stirred for 4 hours, concentrated and the residue was poured into 200 mL of water adjusting the pH to 5 with 1 M HCl. The mixture was stirred for 30 minutes, filtered, and the collected solid was dried in vacuo to give the title compound (6.0 g, 98%).

1. concentrationconcentrated
2. additionthe residue was poured into 200 mL of water adjusting the pH to 5 with 1 M HCl
3. stirringThe mixture was stirred for 30 minutes
4. filtrationfiltered
5. customthe collected solid was dried in vacuo