Water → HCID 10664501, 화합물

HRID 1532805노트

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HRID 1532805 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([C:12]([S:15][CH2:16][CH3:17])([F:14])[F:13])[CH2:11][O:10]1.[NH:18]1[CH:22]=[N:21][CH:20]=[N:19]1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:10])([CH2:11][N:18]1[CH:22]=[N:21][CH:20]=[N:19]1)[C:12]([S:15][CH2:16][CH3:17])([F:14])[F:13]

참가 물질

6

반응물 4

HCID 962WaterHCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 10825624HCID 10825624, 화합물

생성물 1

HCID 10664501HCID 10664501, 화합물수율 28%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
60 °C

실험 절차

To a solution of 2-(2,4-difluorophenyl)-2-[(ethylthio)(difluoro)methyl]oxirane (4.3 g, 0.016 mol) in DMSO (50 ml), 1,2,4-triazole (2.98 g, 0.043 mol) and potassium carbonate (5.96 g, 0.043 mol) were added, followed by stirring at 60° C. for 2 hours. After the completion of the reaction, water was added to the reaction mixture. The resulting mixture was extracted with ethyl acetate. The extract was washed successively with water and saturated saline and dried over magnesium sulfate. The solvent was then distilled off under reduced pressure. The residue so obtained was crystallized from isopropyl ether-ethyl acetate, whereby 2-(2,4-difluorophenyl)-1-(ethylthio)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)-2-propanol (1.5 g, yield: 25%) was obtained as colorless crystals.

후처리

  1. additionwas added to the reaction mixture
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. washThe extract was washed successively with water and saturated saline
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was then distilled off under reduced pressure
  6. customThe residue so obtained
  7. customwas crystallized from isopropyl ether-ethyl acetate

출처 및 근거

ORD 기록
ord-efe73108f61849f4840c5746ffdf1bdb
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06204415B1

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