Ammonia → 4-(4-Nitrophenyl)-morpholin-3-ON

温度

25 °C

In a 2-liter flask, 177 g (1.0 mol) of 4-phenyl-3-morpholinone (VIII) are introduced at internal temperature 10° C. in 4 portions into 728 g (7.4 equivalents) of concentrated sulphuric acid. The mixture is then heated to 25° C. and stirred at this temperature for 30 minutes. The solution is cooled to −5° C. and admixed within one hour with 101.8 g (1.05 equivalents) of 65% nitric acid. The mixture is stirred at −5° C. for one hour. 1300 ml of demineralized water are metered into this solution at 10° C. Subsequently, a pH of 7.4 is established, likewise at 10° C., with 25% aqueous ammonia solution. The suspension is admixed with 2000 g of acetone and heated to 40° C. In the course of this, the product goes into solution, so that the phases can be separated. 1500 g of acetone/water mixture are distilled off at standard pressure from the organic phase, in the course of which the product precipitates out. The suspension is cooled to 10° C. and stirred for a further 30 minutes, and the product is isolated. The moist product is washed with 320 g of cold acetone and dried at 50° C. under reduced pressure.

1. temperatureThe solution is cooled to −5° C.
2. stirringThe mixture is stirred at −5° C. for one hour
3. customare metered into this solution at 10° C
4. temperatureheated to 40° C
5. customcan be separated
6. distillation1500 g of acetone/water mixture are distilled off at standard pressure from the organic phase, in the course of which the product
7. customprecipitates out
8. temperatureThe suspension is cooled to 10° C.
9. stirringstirred for a further 30 minutes
10. customthe product is isolated
11. washThe moist product is washed with 320 g of cold acetone
12. customdried at 50° C. under reduced pressure

ORDレコード

ord-2ae314a9b3a6465b960c704de259a8cf

出典データセット

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07598378B2