Isoamylamine → HCID 22349345、化合物

HRID 896297ノート

反応式

HRID 896297 の反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].[CH2:13]([NH2:18])[CH2:14][CH:15]([CH3:17])[CH3:16]>CN(C=O)C>[CH3:16][CH:15]([CH3:17])[CH2:14][CH2:13][NH:18][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11]

参加物

4

反応物 2

HCID 7894IsoamylamineHCID 13655Benzonitrile, 4-chloro-3-nitro-

生成物 1

HCID 22349345HCID 22349345、化合物収率 90%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-chloro-3-nitrobenzonitrile (18.3 g, 0.10 mol) and isoamylamine (19.2 g, 0.22 mol) in DMF (250 mL) was heated to 90° C. for 4 h under nitrogen then cooled and the solvent evaporated. The residue is triturated with EtOAc (300 mL) and solids removed by filtration. The filtrate was washed with water and brine. The organic layer was dried over MgSO4 and evaporated. The residue was recrystallized from MeOH to give 21.0 g (90%) of 4-(3-methyl-butylamino)-3-nitro-benzonitrile as a yellow crystalline solid.

後処理

  1. temperaturethen cooled
  2. customthe solvent evaporated
  3. customThe residue is triturated with EtOAc (300 mL) and solids
  4. customremoved by filtration
  5. washThe filtrate was washed with water and brine
  6. dry with materialThe organic layer was dried over MgSO4
  7. customevaporated
  8. customThe residue was recrystallized from MeOH

出典と根拠

ORDレコード
ord-f5826d8c5c454360923566cdcc24b79f
出典データセット
uspto-grants-2005_07
特許番号
US06919331B2

反応ノート

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