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Potassium Carbonate → 2-(2,4-Dichlorophenyl)-1-(1,2,4-triazol-1-yl)-3-(5-trifluoromethylimidazol-1-yl)-propan-2-ol

HRID 1583761
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HRID 1583761 반응식
[F:1][C:2]([F:9])([F:8])[C:3]1[N:4]=[CH:5][NH:6][CH:7]=1.S(O)(=O)(=O)C.[Cl:15][C:16]1[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=1[C:23]1([CH2:26][N:27]2[CH:31]=[N:30][CH:29]=[N:28]2)[CH2:25][O:24]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:15][C:16]1[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=1[C:23]([OH:24])([CH2:25][N:4]1[C:3]([C:2]([F:9])([F:8])[F:1])=[CH:7][N:6]=[CH:5]1)[CH2:26][N:27]1[CH:31]=[N:30][CH:29]=[N:28]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 867396002-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonateHCID 178418921HCID 178418921, 화합물

생성물 1

HCID 202583642-(2,4-Dichlorophenyl)-1-(1,2,4-triazol-1-yl)-3-(5-trifluoromethylimidazol-1-yl)-propan-2-ol수율 1%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

A mixture of 4-trifluoromethylimidazole (0.7 g, 5 mmole), 2-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-ylmethyl)-oxirane mesylate salt (1.88 g, 5 mmole) and anhydrous potassium carbonate (2.0 g, 14 mmole) in dry N,N-dimethylformamide (20 ml) was heated at 75°-80° C. for 18 hours. The solvent was evaporated under vacuum and the residue was partitioned between water (20 ml) and methylene chloride (50 ml). The aqueous layer was separated and extracted twice with methylene chloride (30 ml). The organic layers were combined, dried over magnesium sulphate and evaporated to yield the crude product containing the 4- and 5-trifluoromethyl-imidazolyl isomers. The residue was chromatographed on silica eluting with a mixture of hexane, isopropyl alcohol and concentrated ammonium hydroxide (80:20:1.5); fractions containing the minor component were evaporated and the product recrystallised from a mixture of acetone and water to give the desired title compound (0.02 g, 1%), m.p. 190°-192° C.

후처리

  1. temperaturewas heated at 75°-80° C. for 18 hours
  2. customThe solvent was evaporated under vacuum
  3. customthe residue was partitioned between water (20 ml) and methylene chloride (50 ml)
  4. customThe aqueous layer was separated
  5. extractionextracted twice with methylene chloride (30 ml)
  6. dry with materialdried over magnesium sulphate
  7. customevaporated
  8. customto yield the crude product
  9. customThe residue was chromatographed on silica eluting with a mixture of hexane, isopropyl alcohol and concentrated ammonium hydroxide (80:20:1.5)
  10. additionfractions containing the minor component
  11. customwere evaporated
  12. customthe product recrystallised from a mixture of acetone and water

출처 및 근거

ORD 기록
ord-111e71b6ea584342a2b1fd4b45b44227
출처 데이터셋
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04554286

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