Cyclohexylamine → N-cyclohexyl-2-nitroaniline

HRID 220814ノート

反応式

HRID 220814 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 3101179N-cyclohexyl-2-nitroaniline収率 86%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-96a5a38ccfaf44b2938cddca722aa335
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

読み込み中…