实验操作A 10 L double-jacketed reactor was charged with KOtBu (0.22 kg, 1.1equiv) and THF (3 L). The solution was cooled to −20 °C. A mixture of diethyloxalate (260 g, 1 equiv) and 13 (200 g, 1.78 mol, 1.0 equiv) was added below −18 °C. The reaction mixture was stirred at −10 °C for 30 min and then warmed to 15 °C.参考文献Org. Process Res. Dev. 2016, 20, 1637−1646
案例二
最后滴加叔丁醇钾的THF溶液
实验操作A solution of potassium tert-butoxide (32.59 kg, 290.4 mol) in THF (367.5 L) was added dropwise over >2 h to a mixture of 8 (24.50 kg, 138.3mol) and diethyl oxalate (9) (24.25 kg, 138.3 mol) in THF (289.1 L) at 15 to 30 °C, and the resulting mixture was stirred at the same temperature for 1.5 h. After completion of the reaction (confirmed by HPLC Method B), the reaction was quenched with a mixture of hydrochloric acid (35−37%, 10.59kg) and H2O (220.5 L) at <30 °C参考文献https://doi.org/10.1021/acs.oprd.4c00056
案例三
草酸二乙酯和丙酮混合滴加
实验操作A solution of 5.4 M NaOMe in MeOH (507 mL, 1.0equiv) and MeOH (3 L) were heated to 60 °C. A mixture of diethyl oxalate 19 (400 g, 2.737 mol, 1.0 equiv) and acetone (158.75 g, 1.0 equiv) was added to the solution in 25 min. The reaction mixture was stirred at 60 °C for 45 min. 参考文献Org. Process Res. Dev. 2022, 26, 624−634 经验项目
