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2-Methoxyethanol → HCID 23359030, 화합물

HRID 232650
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HRID 232650 반응식
F[C:2]1[C:7]([F:8])=[C:6]([CH3:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:13])[C:3]=1[CH3:14].COCCO.[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>O.C(N(CC)CC)C>[CH3:20][N:21]1[CH2:26][CH2:25][N:24]([C:2]2[C:7]([F:8])=[C:6]([CH3:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:13])[C:3]=2[CH3:14])[CH2:23][CH2:22]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 80192-MethoxyethanolHCID 531671-MethylpiperazineHCID 23358998HCID 23358998, 화합물

생성물 1

HCID 23359030HCID 23359030, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8471Triethylamine용매

실험 절차

To 2,3,6-trifluoro-4-methyl-5-nitrotoluene (1.9 g) are added 2-methoxyethanol (9.9 ml), water (1.1 ml), N-methylpiperazine (4.1 ml) and triethylamine (5.2 ml) and the mixture is refluxed for 25 hours. After the reaction is completed, water is added and the resultant 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 (dichloromethane: methanol=40:1) to give 2-(4-methyl-1-piperazinyl)-3,6-difluoro-4-methyl-5-nitrotoluene (1.73 g).

후처리

  1. temperaturethe mixture is refluxed for 25 hours
  2. extractionthe resultant 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 (dichloromethane: methanol=40:1)

출처 및 근거

ORD 기록
ord-dd48b8fa89aa494daf3de3a8cbca1db2
출처 데이터셋
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05591744

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