Cyclohexylamine → N-cyclohexyl-2-nitroaniline

HRID 220814노트

반응식

HRID 220814 반응식
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH:11]1([NH2:17])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH:11]1([NH:17][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[N+:8]([O-:10])=[O:9])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1

참가 물질

5

반응물 3

HCID 7965CyclohexylamineHCID 11430Potassium CarbonateHCID 738951-Fluoro-2-nitrobenzene

생성물 1

HCID 3101179N-cyclohexyl-2-nitroaniline수율 86%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 2-fluoronitrobenzene (5.0 g, 35.4 mmol), cyclohexylamine (4.5 ml, 39.0 mmol) and potassium carbon-ate (17.1 g, 124 mmol) in acetonitrile (100 ml) was heated at reflux for 2 days. The mixture was diluted with EtOAC, washed with water then brine, dried and partially concentrated in vacuo. The solid which precipitated was collected and washed with hexane to yield the title compound (6.7 g, 86%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 days
  3. additionThe mixture was diluted with EtOAC
  4. washwashed with water
  5. dry with materialbrine, dried
  6. concentrationpartially concentrated in vacuo
  7. customThe solid which precipitated
  8. customwas collected
  9. washwashed with hexane

출처 및 근거

ORD 기록
ord-96a5a38ccfaf44b2938cddca722aa335
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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