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

HRID 1670368
ノート
印刷プレビュー

反応式

HRID 1670368 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8e735db6e981406bb4caae1efa0c81d8
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07994094B2

反応ノート

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