反应详情

温度

85 °C

102.6 g of moist paste of 2-chloro-5-nitrophenyl 2-hydroxyethyl sulphone from Example 1 [or an equimolar amount of 4-chloro-3-nitrophenyl 2-hydoxyethyl sulphone] are stirred into 250 ml of water and 50 ml of the phosphate buffer solution described under Example 2. A small amount of a nonionic emulsifier and 5 g of palladium-oncharcoal catalyst are added. Hydrogenation with hydrogen is then carried out in an autoclave at 70° C. and approximately 40 bar. The reduction is monitored by chromatography. After the hydrogenation, and after releasing the pressure and flushing the reactor, the product is heated to 85° C. and clarified via a pressure filter. The filter is cooled to 0° C. and the crystalline 3-aminophenyl 2-hydroxyethyl sulphone is isolated by filtration. 53 g of single-substance product are obtained after drying.

1. customis then carried out in an autoclave at 70° C.
2. customflushing the reactor
3. filtrationfilter
4. temperatureThe filter is cooled to 0° C.