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

HRID 231361

反応式

HRID 231361 の反応式
[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

参加物

4

反応物 3

HCID 6492DicyclopentadieneHCID 72612,4-DiaminotolueneHCID 8003Pentane

生成物 1

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

反応条件

温度
205 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f9d2888bf0c343fc99e299bc562e2391
出典データセット
uspto-grants-1989_07
特許番号
US04845291

関連ノート

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