Cyclohexylamine → 1H-Pyrrole, 1-cyclohexyl-2,5-dihydro-

HRID 126908

반응식

HRID 126908 반응식
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[CH:9]=[CH:10][CH2:11][CH2:12]Cl>C1C=CC=CC=1>[CH:1]1([N:7]2[CH2:12][CH:11]=[CH:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 7965CyclohexylamineHCID 35801CID 35801

생성물 1

HCID 1065901H-Pyrrole, 1-cyclohexyl-2,5-dihydro-수율 76%

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
92 °C

실험 절차

A solution of 5.19 kg (52.3 moles) of cyclohexylamine in 4.0 liters of benzene was heated to mild reflux (92° C.) and then the heating discontinued. To the solution was added, dropwise, 1,635 g (13.1 moles) of 1,4-dichlorobutene at a rate sufficient to maintain gentle reflux, 3 hours time being required. Heat was reapplied and the reactants were heated at reflux temperature for 18 hours. The mixture was cooled to about 50° C. and filtered to remove the hydrochloride. Carbon dioxide was bubbled into the filtrate to precipitate excess amine carbonate which was removed by filtration. Solvent was removed from the filtrate by distillation under reduced pressure and the reddish fluid residue slightly contaminated with benzene weighed 1,506 g (76% yield).

후처리

  1. additionTo the solution was added
  2. temperatureHeat
  3. temperaturethe reactants were heated
  4. temperatureat reflux temperature for 18 hours
  5. temperatureThe mixture was cooled to about 50° C.
  6. filtrationfiltered
  7. customto remove the hydrochloride
  8. customCarbon dioxide was bubbled into the filtrate
  9. customto precipitate excess amine carbonate which
  10. customwas removed by filtration
  11. customSolvent was removed from the filtrate by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-b377109ab96d469c846532b1cff41539
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254135

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