反应详情

温度

100 °C

To a solution of the product of Example 39-4 (320 g, 1.01 mol) in toluene (1100 mL) was added product of Example 17A-4 (291 g, 1.01 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 (472, 4.66 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 (2000 mL) was added. The organic layer was washed with 10% KH2PO4 and 10% NaCl then concentrated to a thick oil then chased with CH2Cl2. The crude product of Example 39-5 (assay for 406.5 g, 74.5%) was used directly.

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