反应详情

温度

7.5 °C

To the so obtained solution, a solution of the acetylsalicylic acid chloride (16 g, 0.08 moles) in toluene (50 ml) is added under stirring at the temperature of 5-10° C. The mixture is maintained at a temperature within the above range, under stirring for 2 hours, then poured into water and then extracted with dichloromethane (2×100 ml). The organic phase is separated, washed in sequence with a solution of potassium carbonate at 25% w/v, with water, with a 3% hydrochloric acid solution and finally again with water, then anhydrified with sodium sulphate and the solvent evaporated under reduced pressure. The residue is crystallized from isopropanol. 3-hydroxymethyl phenyl ester of the 2-acetoxybenzoic acid (45.8 g, 0.16 moles, yield 80%) is obtained.

1. temperatureThe mixture is maintained at a temperature within the above range
2. stirringunder stirring for 2 hours
3. extractionextracted with dichloromethane (2×100 ml)
4. customThe organic phase is separated
5. washwashed in sequence with a solution of potassium carbonate at 25%
6. customthe solvent evaporated under reduced pressure
7. customThe residue is crystallized from isopropanol