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

HRID 900839

반응식

HRID 900839 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-32428475ae3e40a3b5eaaa00620bcfc6
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07361675B2

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