反应详情

温度

12.5 °C

Thionyl chloride (13.8 ml) was added over ˜15 minutes to a stirred solution of ethyl 6-(hydroxymethyl)-2-pyridinecarboxylate (28.5 g) in MDC (200 ml) maintaining the temperature at 10-15° C. using an ice-water bath. On completion of the addition the mixture was stirred at room temperature for 1 hour. The solvent was evaporated and the residue partitioned between toluene (200 ml)/saturated bicarb (sodium bicarbonate solution, 200 ml). The layers were separated and the organic phase washed with water (150 ml). The solvent was evaporated to leave a pale oil which solidified on standing. (31.3 g).

1. additionOn completion of the addition the mixture
2. customThe solvent was evaporated
3. customthe residue partitioned between toluene (200 ml)/saturated bicarb (sodium bicarbonate solution, 200 ml)
4. customThe layers were separated
5. washthe organic phase washed with water (150 ml)
6. customThe solvent was evaporated
7. customto leave a pale oil which