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Thionyl Chloride → 1-(4-Fluorophenyl)-4-methyl-5-chloromethyl-1,2,3-triazole

HRID 1090116
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HRID 1090116 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([CH2:13]O)=[C:11]([CH3:15])[N:10]=[N:9]2)=[CH:4][CH:3]=1.S(Cl)([Cl:18])=O>C1C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([CH2:13][Cl:18])=[C:11]([CH3:15])[N:10]=[N:9]2)=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 19914681(1-(4-Fluorophenyl)-4-methyl-1H-1,2,3-triazol-5-yl)methanol

생성물 1

HCID 199146751-(4-Fluorophenyl)-4-methyl-5-chloromethyl-1,2,3-triazole

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 1-(4-fluorophenyl)-4-methyl-5-hydroxymethyl-1,2,3-triazole (871 mg; 4.20 mmol), prepared as described in example 6, and thionyl chloride (400 ml; 5.46 mmol) in benzene (14 ml) was heated under reflux for 4 hours. The reaction mixture was kept under stirring at room temperature overnight, thionyl chloride and benzene were evaporated and the resultant crude compound was collected several times with benzene. After evaporation of the solvent, the crude compound was purified by chromatography on silica gel (230-400 mesh), eluent methylene chloride:acetone=95:5, giving the title compound (m.p. 70°-71° C.).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. customthionyl chloride and benzene were evaporated
  4. customthe resultant crude compound was collected several times with benzene
  5. customAfter evaporation of the solvent
  6. customthe crude compound was purified by chromatography on silica gel (230-400 mesh), eluent methylene chloride

출처 및 근거

ORD 기록
ord-dce0ef16f7bd487a8ff610c1e8344581
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05081136

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