Ammonia → Prodiamine

HRID 2071241

반응식

HRID 2071241 반응식
[CH2:1]([N:4]([CH2:22][CH2:23][CH3:24])[C:5]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([C:14]([F:17])([F:16])[F:15])=[C:7](Cl)[C:6]=1[N+:19]([O-:21])=[O:20])[CH2:2][CH3:3].[NH3:25]>C(O)C>[CH2:1]([N:4]([CH2:22][CH2:23][CH3:24])[C:5]1[C:6]([N+:19]([O-:21])=[O:20])=[C:7]([NH2:25])[C:8]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[CH2:2][CH3:3]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 94399Benzenamine, 3-chloro-2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)-

생성물 1

HCID 34469Prodiamine

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

A glass reaction tube was charged with 4.0 grams (0.0108 mole) of N,N-di-n-propyl-3-chloro-2,6-dinitro-4-trifluoromethylaniline, 5.82 grams (0.0237 mole) of 6.95% ethanolic ammonia and 35 ml. of ethanol. The tube was sealed and heated in an oven at 100° C. for 68 hours. The contents of the tube were cooled and the ethanol removed by evaporation. Water was added to the solid orange residue to dissolve the ammonium chloride and the insoluble produced was separated by filtration. The product was dissolved in refluxing 95% ethanol. Upon cooling, orange needles and a yellow powder crystallized. The yellow powder was identified as 2,4-dinitro-6-trifluoromethyl-1,3-phenylenediamine and was separated from the desired product by filtration after extracting with boiling hexane. The desired product dissolved in the hexane and was isolated from the filtrate by evaporation of the hexane. The residue was recrystallized from 95% ethanol to give orange needles, m.p. 124°-125° C.

후처리

  1. customA glass reaction tube
  2. customThe tube was sealed
  3. temperatureThe contents of the tube were cooled
  4. customthe ethanol removed by evaporation
  5. additionWater was added to the solid orange residue
  6. dissolutionto dissolve the ammonium chloride
  7. customthe insoluble produced
  8. customwas separated by filtration
  9. dissolutionThe product was dissolved
  10. temperaturein refluxing 95% ethanol
  11. temperatureUpon cooling
  12. customorange needles and a yellow powder crystallized
  13. customwas separated from the desired product by filtration
  14. extractionafter extracting with boiling hexane
  15. dissolutionThe desired product dissolved in the hexane
  16. customwas isolated from the filtrate by evaporation of the hexane
  17. customThe residue was recrystallized from 95% ethanol
  18. customto give orange needles, m.p. 124°-125° C.

출처 및 근거

ORD 기록
ord-e59f9dfbcc2f4b3aa917c89a9f03d7ce
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046758

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