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

HRID 1817782

반응식

HRID 1817782 반응식
[C:1]1([N:7]2[CH2:12][CH2:11][O:10][CH2:9][C:8]2=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.[N+:19]([O-])([OH:21])=[O:20].N>CC(C)=O.O>[N+:19]([C:4]1[CH:3]=[CH:2][C:1]([N:7]2[CH2:12][CH2:11][O:10][CH2:9][C:8]2=[O:13])=[CH:6][CH:5]=1)([O-:21])=[O:20]

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 51530804-Phenylmorpholin-3-ON

생성물 1

HCID 114473754-(4-Nitrophenyl)-morpholin-3-ON

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ae314a9b3a6465b960c704de259a8cf
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07598378B2

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