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Methanol → 4-Methyl-3-methylsulfonyl-5-phenyl-4H-1,2,4-triazole

HRID 252635
ノート
印刷プレビュー

反応式

HRID 252635 の反応式
[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:5][N:4]=[C:3]1SC.O[O:16][S:17]([O-:19])=O.[K+].[CH3:21]O>>[CH3:1][N:2]1[C:6]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[N:5][N:4]=[C:3]1[S:17]([CH3:21])(=[O:19])=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 2132261H-1,2,4-Triazole, 4-methyl-3-(methylthio)-5-phenyl-HCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 1640134-Methyl-3-methylsulfonyl-5-phenyl-4H-1,2,4-triazole

実験手順

A slurry of 4-methyl-3-(methylthio)-5-phenyl-4H-1,2,4-triazole (0.360 g, 1.75 mmol) and oxone(r) monopersulfate compound (2.16 g, 3.51 mmol) were stirred rapidly in 5 mL MeOH overnight. The reaction was concentrated and the solids diluted with water, ice, and treated with 6 N NaOH until a pH>10. The resulting material was extracted 3×DCM, and the combined organic layers were dried over anhyd sodium sulfate, filtered, and concentrated to give 4-methyl-3-(methylsulfonyl)-5-phenyl-4H-1,2,4-triazole as a white solid. MS m/z=238 [M+H]+. Calc'd for C10H11N3O2S: 237.3.

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  1. concentrationThe reaction was concentrated
  2. additionthe solids diluted with water, ice
  3. additiontreated with 6 N NaOH until a pH>10
  4. extractionThe resulting material was extracted 3×DCM
  5. dry with materialthe combined organic layers were dried over anhyd sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-101126bfd1b347458ea7c06869a33c1d
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07868177B2

反応ノート

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