Dicyclopentadiene → 4-(Cyclopent-2-en-1-yl)-6-methylbenzene-1,3-diamine

HRID 231361

반응식

HRID 231361 반응식
[C:1]1([CH3:9])[C:2]([NH2:8])=[CH:3][C:4]([NH2:7])=[CH:5][CH:6]=1.C1C2C3C=CC(C2C=C1)C3.[CH3:20][CH2:21][CH2:22][CH2:23][CH3:24]>>[CH:22]1([C:5]2[CH:6]=[C:1]([CH3:9])[C:2]([NH2:8])=[CH:3][C:4]=2[NH2:7])[CH2:23][CH2:24][CH:20]=[CH:21]1

참가 물질

4

반응물 3

HCID 6492DicyclopentadieneHCID 72612,4-DiaminotolueneHCID 8003Pentane

생성물 1

HCID 140698844-(Cyclopent-2-en-1-yl)-6-methylbenzene-1,3-diamine

반응 조건

온도
205 °C

실험 절차

A 200g (1.64 mol) portion of 2,4-toluenediamine, 162g (1.23 mol, 2,45 equiv) of dicyclopentadiene, 200g (2.78 mol) of pentane, and 20.0g of an amorphous alumina-silica catalyst comprised of 13% alumina and 87% silica were charged to a 1000cc pressure vessel equipped with a mechanical stirrer. The vessel was sealed and purged with nitrogen leaving a 32 psig nitrogen blanket. The vessel contents were heated to 205° C. with stirring and were maintained at that temperature for 22 hours. The contents were cooled to 150° C. and isolated catalyst free by hot filtration. Selective removal of residual hydrocarbons by vacuum distillation and analysis by gas chromatography (GC) provides the following product mixture.

후처리

  1. additionwere charged to a 1000cc pressure vessel
  2. customequipped with a mechanical stirrer
  3. customThe vessel was sealed
  4. custompurged with nitrogen leaving a 32 psig nitrogen blanket
  5. temperaturewere maintained at that temperature for 22 hours
  6. temperatureThe contents were cooled to 150° C.
  7. customisolated catalyst
  8. filtrationfree by hot filtration
  9. customremoval of residual hydrocarbons
  10. distillationby vacuum distillation and analysis by gas chromatography (GC)
  11. customprovides the following product mixture

출처 및 근거

ORD 기록
ord-f9d2888bf0c343fc99e299bc562e2391
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845291

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