Methyl iodide → 3-(2,6-Dichloro-4-trifluoromethylphenyl)-1-methyl-5-methylsulfenylpyrazole

HRID 1598512ノート

反応式

HRID 1598512 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[C:13]1[CH:17]=[C:16]([SH:18])[N:15]([CH3:19])[N:14]=1.CI.[C:22](=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:9])([F:11])[F:10])[CH:5]=[C:4]([Cl:12])[C:3]=1[C:13]1[CH:17]=[C:16]([S:18][CH3:22])[N:15]([CH3:19])[N:14]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178481742HCID 178481742、化合物

生成物 1

HCID 189294193-(2,6-Dichloro-4-trifluoromethylphenyl)-1-methyl-5-methylsulfenylpyrazole収率 97.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A suspension of 0.5 g of 3-(2,6-dichloro-4-trifluoromethylphenyl)-5-mercapto-1-methylpyrazole (2), 2.3 g of methyl iodide and 0.4 g of anhydrous potassium carbonate in 10 ml of acetonitrile was refluxed overnight with stirring. The reaction mixture was cooled to room temperature and filtered through Celite, and the filtrate was concentrated under reduced pressure. The residue was purified by chromatography on silica gel to obtain 0.51 g of the desired product in the form of white crystals.

後処理

  1. temperaturewas refluxed overnight
  2. filtrationfiltered through Celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-d64ec6771ae04d188fa3214f745faab4
出典データセット
uspto-grants-1998_04
特許番号
US05739083

反応ノート

読み込み中…