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Water → HCID 15453099, 화합물

HRID 611816
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HRID 611816 반응식
[F:1][C:2]([F:21])([S:19][CH3:20])[C:3]([C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[F:18])([OH:10])[CH2:4][N:5]1[CH:9]=[N:8][CH:7]=[N:6]1.ClC1C=CC=C(C(OO)=[O:30])C=1.O>C(Cl)Cl>[F:21][C:2]([F:1])([S:19]([CH3:20])=[O:30])[C:3]([C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[F:18])([OH:10])[CH2:4][N:5]1[CH:9]=[N:8][CH:7]=[N:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 10853188HCID 10853188, 화합물

생성물 1

HCID 15453099HCID 15453099, 화합물수율 40.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a 10 ml solution of 150 mg (0.47 mmol) of 3,3-difluoro-2-(2',4'-difluorophenyl)-3-methylthio-1-(1H-1,2,4-triazol-1-yl)propan-2-ol [Compound (1a-1)] in methylene chloride, 114 mg (0.56 mmol) of m-chloroperbenzoic acid were added at room temperature, followed by stirring for 30 minutes. To the reaction mixture, water was added, followed by extraction with chloroform. The extract was then washed successively with a 10% aqueous solution of sodium thiosulfate and a 10% aqueous solution of sodium carbonate, followed by drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The oil so obtained was purified by chromatography on a silica gel column using chloroform:methanol (10:1), whereby 64 mg of the title Compound (1b-1) [diastereomers (1b-1A):(1b-1B)=2.5:1] were obtained in the form of colorless crystals (yield: 403).

후처리

  1. extractionfollowed by extraction with chloroform
  2. washThe extract was then washed successively with a 10% aqueous solution of sodium thiosulfate
  3. dry with materialby drying over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customThe oil so obtained
  6. customwas purified by chromatography on a silica gel column

출처 및 근거

ORD 기록
ord-0f9ab13e4e6e4d9ca47a29c247fae463
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06002028

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