Dithiocarbamates (DTCs)主要以下三种,这三种配体可以和过渡金属形成溶解度不好的螯合物,过滤去除过渡金属。
APDTC应用案例一(除钯的吸附法)
实验操作
Following these aqueous washes, to the organic phase in R1, was added APDTC (ammonium pyrrolidine dithiocarbamate, 1.30 kg, 7.91 mol, 0.061 equiv, 0.030X) and purified water (0.28 kg, 15 mol, 0.12 equiv), then the mixture was adjusted to 45−55 °C and stirred for about 2 h.
The mixture was filtered and washed with 2-MeTHF (60 kg, 1.5 mL/g), and to the filtrate (assayed to contain ∼1375 ppm [Pd]) was added additional APDTC (1.40 kg, 8.52 mol, 0.066 equiv, 0.030X) and additional water (0.30 kg, 17 mol, 0.13 equiv). The mixture was again heated to 45−55 °C and stirred for about 3 h and then filtered and washed with 2-MeTHF (80 kg, 2.0 mL/g). The filtrate (assayed to contain ∼155 ppm [Pd]) was added back into R1
参考文献
https://doi.org/10.1021/acs.oprd.4c00162
APDTC应用案例二(吸附法)
实验操作
Once complete by HPLC, the reaction was cooled to 50 °C. A solution of KOH (0.68 equiv, 12.8 kg) in EtOH (229 L) was added followed by ammonium pyrrolidinedithiocarbamate (0.68 equiv, 39.4 kg). The mixture was allowed to stir at 50 °C for 1 h. The mixture was then filtered over a bed of Celite followed by an in-line polish filter (1 μm).
参考文献
DOI: 10.1021/acs.oprd.7b00191