Ethanol → HCID 23359031、化合物

HRID 2396961ノート

反応式

HRID 2396961 の反応式
F[C:2]1[C:7]([F:8])=[C:6]([Cl:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:13])[C:3]=1[CH3:14].C(O)C.[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>O.C(N(CC)CC)C>[CH3:18][N:19]1[CH2:24][CH2:23][N:22]([C:2]2[C:7]([F:8])=[C:6]([Cl:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:13])[C:3]=2[CH3:14])[CH2:21][CH2:20]1

参加物

6

反応物 3

HCID 702EthanolHCID 531671-MethylpiperazineHCID 23358995HCID 23358995、化合物

生成物 1

HCID 23359031HCID 23359031、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8471Triethylamine溶媒

実験手順

To 2,3,6-trifluoro-4-chloro-5-nitrotoluene (0.17 g) are added ethanol (3.3 ml), water (0.5 ml), N-methylpiperazine (0.45 ml) and triethylamine (0.56 ml) and the mixture is refluxed for 24 hours. After the reaction is completed, water is added to the reaction mixture and the mixture is extracted with diethyl ether, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (eluent; dichloromethane: methanol=20 : 1) to give 2-(4-methyl-1-piperazinyl)-3,6-difluoro-4-chloro-5-nitrotoluene (0.13 g).

後処理

  1. temperaturethe mixture is refluxed for 24 hours
  2. extractionthe mixture is extracted with diethyl ether
  3. washthe extract is washed with water
  4. customdried
  5. distillationThe solvent is distilled off under reduced pressure
  6. customthe residue is purified by silica-gel column-chromatography (eluent; dichloromethane: methanol=20 : 1)

出典と根拠

ORDレコード
ord-40d4326fb4b54cc99073f5bb89638d1d
出典データセット
uspto-grants-1996_02
特許番号
US05495020

反応ノート

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