反应详情

温度

90 °C

The compound 3 is suspended in toluene and heated to 80-100° C. After addition of 1.5 equivalents phosphorus oxychloride the mixture is heated for 6 hours to 80-100° C. and then cooled within 3 hours to 20° C. The suspension is added to water while maintaining the pH of the aqueous layer during addition and subsequent stirring between 7-8 by addition of a sodium hydroxide solution. The mixture is stirred until all precipitate is dissolved. After phase separation the water is removed by azeotropic distillation. Then 1.0 equivalent of methanesulfonic acid is added and the formed suspension stirred for some time. At this point in time parts of the solvent may be replaced by acetone, and then the mixture is slowly cooled to 0-10° C. and stirred at this temperature for another couple of hours. After filtration the product is washed with toluene and dried in vacuo.

1. temperatureis heated for 6 hours to 80-100° C.
2. temperaturecooled within 3 hours to 20° C
3. temperaturewhile maintaining the pH of the aqueous layer
4. additionduring addition
5. dissolutionis dissolved
6. customAfter phase separation the water
7. customis removed by azeotropic distillation
8. stirringthe formed suspension stirred for some time
9. temperaturethe mixture is slowly cooled to 0-10° C.
10. stirringstirred at this temperature for another couple of hours
11. filtrationAfter filtration the product
12. washis washed with toluene
13. customdried in vacuo