反应详情

The propan-2-ol (38.2 mL, 499 mmol) was added drop wise over 15 min to a cold (0° C.), nitrogen purged solution of oxalyl dichloride (101 g, 799 mmol) and the reaction was stirred at room temperature for 2.5 h. Then a reflux condenser was fitted and a slight vacuum was applied for about 1 h until HCl gas was removed (the HCl was trapped in by a sat'd solution of NaHCO3). The reflux condenser was removed and the flask was fitted with a short path distillation head. Excess reagent was removed by distillation under house vacuum (oil bath heated to 65° C.), and then the temperature was raised to between 85-95° C. and the product was distilled (NOTE: The 1st fraction of ˜5 mL was discarded) to provide isopropyl 2-chloro-2-oxoacetate 52.62 g (70%).

1. customThen a reflux condenser was fitted
2. customwas removed (the HCl
3. customThe reflux condenser was removed
4. customthe flask was fitted with a short path distillation head
5. customExcess reagent was removed by distillation under house vacuum (oil bath heated to 65° C.)
6. temperaturethe temperature was raised to between 85-95° C.
7. distillationthe product was distilled (NOTE