Stannane, trimethylphenyl- → 3-Methylthio-5-phenyl-1,2,4-thiadiazole

HRID 900839

反応式

HRID 900839 の反応式
Cl[C:2]1[S:6][N:5]=[C:4]([S:7][CH3:8])[N:3]=1.C[Sn](C)(C)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[F-].[K+]>C1(C)C=CC=CC=1>[CH3:8][S:7][C:4]1[N:3]=[C:2]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[S:6][N:5]=1

参加物

5

反応物 3

HCID 123095Stannane, trimethylphenyl-HCID 522689Potassium FluorideHCID 5709535-Chloro-3-(methylsulfanyl)-1,2,4-thiadiazole

生成物 1

HCID 230869103-Methylthio-5-phenyl-1,2,4-thiadiazole収率 72.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To 30 ml of toluene were added 500 mg of 5-chloro-3-methylthio-1,2,4-thiadiazole, 794 mg of trimethylphenyltin and 346 mg of tetrakistriphenylphosphine palladium, and the mixture was heated under reflux for 8 hours in a nitrogen atmosphere. Then, the reaction mixture was cooled to room temperature, and a 20% aqueous potassium fluoride solution was added to the reaction mixture, followed by stirring. This mixture was filtered through Celite, and the filtrate was concentrated. The resulting residue was subjected to silica gel column chromatography to obtain 455 mg of 3-methylthio-5-phenyl-1,2,4-thiadiazole.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 8 hours in a nitrogen atmosphere
  3. filtrationThis mixture was filtered through Celite
  4. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-32428475ae3e40a3b5eaaa00620bcfc6
出典データセット
uspto-grants-2008_04
特許番号
US07361675B2

関連ノート

読み込み中…