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1H-1,2,4-Triazole → HCID 15433416, 화합물

HRID 613394
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HRID 613394 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([O:19][CH2:18]1)[C:10]([F:17])([F:16])[S:11][CH2:12][CH2:13][O:14][CH3:15].[NH:20]1[CH:24]=[N:23][CH:22]=[N:21]1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.CCOCC>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:19])([CH2:18][N:20]1[CH:24]=[N:23][CH:22]=[N:21]1)[C:10]([F:17])([F:16])[S:11][CH2:12][CH2:13][O:14][CH3:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 154343832-(2,4-Difluorophenyl)-1,1-difluoro-1-(2-methoxyethyl)thio-2,3-epoxypropane

생성물 1

HCID 15433416HCID 15433416, 화합물수율 12.4%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 3283
Diethyl Ether
용매

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온도
50 °C

실험 절차

To a solution of 2-(2,4-difluorophenyl)-1,1-difluoro-1-[(2-methoxyethyl)thio]-2,3-epoxypropane (13.0 g, 0.044 mol) in DMSO (100 ml), 1,2,4-triazole (7.6 g, 0.11 mol) and potassium carbonate (15.2 g, 0.11 mol) were added and the resulting mixture was stirred at room temperature for 12 hours and at an external temperature of 50° C. for one hour. After the completion of the reaction, the reaction mixture was diluted with ether and insoluble matter was filtered off. The ether solution was washed with water, dried over magnesium sulfate and distilled off under reduced pressure. The residue was recrystallized from isopropyl ether-ethyl acetate, whereby 2-(2,4-difluorophenyl)-1,1-difluoro-1-[(2-methoxyethyl)thio]-3-(1H-1,2,4-triazol-1-yl)-2-propanol (2.0 g, yield: 12.0%) was obtained as colorless crystals.

후처리

  1. customAfter the completion of the reaction
  2. filtrationwas filtered off
  3. washThe ether solution was washed with water
  4. dry with materialdried over magnesium sulfate
  5. distillationdistilled off under reduced pressure
  6. customThe residue was recrystallized from isopropyl ether-ethyl acetate

출처 및 근거

ORD 기록
ord-15fd9a3188044b8b8f147b93b4373b2a
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06008239

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