Isopropylamine → N-Isopropyl-3,4-dimethyl-2,6-dinitroaniline

HRID 261276노트

반응식

HRID 261276 반응식
Cl[C:2]1[C:3]([N+:13]([O-:15])=[O:14])=[C:4]([CH3:12])[C:5]([CH3:11])=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[CH:16]([NH2:19])([CH3:18])[CH3:17]>>[CH:16]([NH:19][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([CH3:11])=[C:4]([CH3:12])[C:3]=1[N+:13]([O-:15])=[O:14])([CH3:18])[CH3:17]

참가 물질

3

반응물 2

HCID 6363IsopropylamineHCID 134551024-Chloro-3,5-dinitro-o-xylene

생성물 1

HCID 12767671N-Isopropyl-3,4-dimethyl-2,6-dinitroaniline수율 80%

실험 절차

4-Chloro-3,5-dinitro-o-xylene (10.0 grams, 0.043 mole) and i-propylamine (10.1 grams, 0.17 mole) are mixed and refluxed for 12 hours using an efficient reflux condenser. The mixture is then cooled and poured into 100 ml. of 5% hydrochloric acid and extracted with diethyl ether. The ether extract is dried over magnesium sulfate. Removal of the drying agent and solvent leaves an orange oil which readily solidifies. The product is recrystallized from methanol to give 8.7 grams (80%) of an orange solid with melting point 69° C. to 70° C.

후처리

  1. temperaturerefluxed for 12 hours
  2. temperatureThe mixture is then cooled
  3. additionpoured into 100 ml
  4. extractionof 5% hydrochloric acid and extracted with diethyl ether
  5. extractionThe ether extract
  6. dry with materialis dried over magnesium sulfate
  7. customRemoval of the drying agent and solvent
  8. customleaves an orange oil which
  9. customThe product is recrystallized from methanol

출처 및 근거

ORD 기록
ord-7c3f4e65f59046218b88437fa1a62074
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04165231

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