反应详情

温度

100 °C

To a solution of the product of Example 49-4 (330.1 g, 0.999 mol) in toluene (1500 mL) was added the product of Example 17A-4 (287.1 g, 0.999 mol). The solution was heated to 100° C. for 4 h then cooled to RT. The solution was transferred to a pressure bottle and triethylamine (505.4, 4.99 mol) was added and the solution was heated to 100° C. for 26 h. The solution was concentrated to ⅓ of the original volume and ethyl acetate (1500 mL) was added. The organic layer was washed with 10% KH2PO4 and 10% NaCl then concentrated to a thick oil then chased with dichloromethane. The crude title compound (assay for 375.8 g, 68%) was used directly in the next step.

1. temperaturethen cooled to RT
2. additionwas added
3. temperaturethe solution was heated to 100° C. for 26 h
4. concentrationThe solution was concentrated
5. additionwas added
6. washThe organic layer was washed with 10% KH2PO4 and 10% NaCl
7. concentrationthen concentrated to a thick oil