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Methyl iodide → 1-Methyl-5-methylthio-3-(trifluoromethyl)pyrazole

HRID 1670368
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HRID 1670368 반응식
[CH3:1][N:2]1[C:6](=[S:7])[CH:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[NH:3]1.[C:12](=O)([O-])[O-].[K+].[K+].CI>C(#N)C>[CH3:1][N:2]1[C:6]([S:7][CH3:12])=[CH:5][C:4]([C:8]([F:11])([F:9])[F:10])=[N:3]1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 190676872-Methyl-5-trifluoromethyl-2H-pyrazole-3-thiol

생성물 1

HCID 593563841-Methyl-5-methylthio-3-(trifluoromethyl)pyrazole수율 86.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

3.87 g of compound (8-5) and 4.40 g of potassium carbonate were suspended in 100 ml of acetonitrile. The suspension was stirred at room temperature for 15 minutes. A solution of 3.62 g of methyl iodide in 10 ml of acetonitrile was added dropwise, and the mixture was stirred at room temperature for 12 hours. The reaction solution was concentrated under reduced pressure. After water was added to the residue, the mixture was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure to produce 3.60 g of 1-methyl-5-methylthio-3-(trifluoromethyl)pyrazole (14).

후처리

  1. stirringthe mixture was stirred at room temperature for 12 hours
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additionAfter water was added to the residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8e735db6e981406bb4caae1efa0c81d8
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07994094B2

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