Ethanol → HCID 23359031, 화합물

HRID 2396961노트

반응식

HRID 2396961 반응식
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

참가 물질

6

반응물 3

HCID 702EthanolHCID 531671-MethylpiperazineHCID 23358995HCID 23358995, 화합물

생성물 1

HCID 23359031HCID 23359031, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8471Triethylamine용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-40d4326fb4b54cc99073f5bb89638d1d
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05495020

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