Ethanol → HCID 23359031, 화합물

HRID 232666노트

반응식

HRID 232666 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-methyl-piperazine (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-a11e228301d64d1ca8a12148506daa14
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591744

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