反应详情

In a 2 liter, 3-neck flask equipped with a water bath, stirrer and thermometer is placed 200 ml of thionyl chloride (2.75 mols). To this is added about half the 360 g (2 mols) of aspirin. The fairly mobile suspension is stirred and warmed to 30° and 4 g of urea then added. Initiation of the reaction appears to be enhanced by minimal agitation. Evolution of HCl gas, and a fairly rapid fall in temperature indicate that the reaction has started, and a slow to medium stirring rate is then maintained. The temperature of the mixture is held at 25°. As mobility increases the remaining aspirin is fed in via a powder funnel in the third neck of the flask, fitted with a `Y` piece, one arm leading to a gas outlet connected to a scrubber for absorbing HCl and SO2. It is important to avoid the ingress of air containing moisture during this stage of the reaction. The completion of the reaction is indicated by the appearance of the reaction mixture which becomes a clear pale yellow fluid. At this stage a further 30 mins stirring at 25°-30° is given. This is followed by the addition of approximately 500 ml of 60°-80° petroleum ether at ca 30° with vigorous stirring. On cooling, the acid chloride is thrown out of solution as a heavy crystalline off-white solid. It is filtered off, washed with petroleum ether and dried quickly in a forced draught oven at 35°-40°. Exposure to air should be kept to a minimum.

1. customIn a 2 liter, 3-neck flask equipped with a water bath, stirrer
2. temperaturewarmed to 30°
3. temperaturea slow to medium stirring rate is then maintained
4. customis held at 25°
5. customis fed in via a powder funnel in the third neck of the flask
6. customfitted with a `Y` piece, one arm
7. customleading to a gas outlet
8. customfor absorbing HCl and SO2
9. additioncontaining moisture
10. customduring this stage of the reaction
11. stirringAt this stage a further 30 mins stirring at 25°-30°
12. temperatureOn cooling
13. filtrationIt is filtered off
14. washwashed with petroleum ether
15. customdried quickly in a forced draught oven at 35°-40°