反应详情

温度

0 °C

A stirred solution of Example 1A (3.48 g, 15.0 mmol) in CH2Cl2 (60 mL) at 0° C. was treated with pyridine (1.20 mL). The reaction mixture was treated dropwise with thionyl chloride (1.10 mL, 15.0 mmol), and the reaction flask was equipped with a calcium chloride drying tube. The reaction mixture was stirred at 0° C. for 4 hours, the cooling bath was removed, and the solution was stirred at ambient temperature for an additional 12 hours. Concentration of the reaction mixture provided a white solid which was triturated with diethyl ether (2×200 mL) to provide 2.40 g of the desired product as a white solid.

1. customthe reaction flask was equipped with a calcium chloride drying tube
2. customthe cooling bath was removed
3. stirringthe solution was stirred at ambient temperature for an additional 12 hours
4. customConcentration of the reaction mixture provided a white solid which
5. customwas triturated with diethyl ether (2×200 mL)