Isoamylamine → HCID 22349345, 화합물

HRID 896297노트

반응식

HRID 896297 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 22349345HCID 22349345, 화합물수율 90%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f5826d8c5c454360923566cdcc24b79f
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06919331B2

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