Tetrahydrofuran → HCID 178504852、化合物

HRID 1011495ノート

反応式

HRID 1011495 の反応式
CS[C:3]1[NH:7][CH:6]=[N:5][N:4]=1.[S:8]([O-:13])(O[O-])(=O)=[O:9].[K+].[K+].[CH2:16]1COCC1>O>[CH3:16][S:8]([C:3]1[N:7]=[CH:6][NH:5][N:4]=1)(=[O:13])=[O:9]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 5753783-Methylthio-4H-1,2,4-triazoleHCID 10313463Potassium peroxymonosulphate

生成物 1

HCID 178504852HCID 178504852、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred solution of 3-methylthio-4H-1,2,4-triazole (1.00 g; Oakwood Products, Inc., West Columbia, S.C.) in THF (20 mL) and water (20 mL) was added potassium peroxomonosulfate (Oxone®, DuPont Specialty Chemicals, Deepwater, N.J., USA) (10.7 g). After stirring at room temperature for a day, the reaction mixture was filtered and the filtercake was washed with THF. The filtrate was partitioned between water and ethyl acetate, the bilayer was separated and the aqueous portion was extracted twice with ethyl acetate. The combined organic extracts were dried over MgSO4, filtered, and the filtrate concentrated under reduced pressure. The resulting residue was purified by flash chromatography (SiO2, ethyl acetate/methanol, 0-10%) to afford 0.496 g of (I-5a) as a white solid. m/z 148.1 (M+H)+.

後処理

  1. filtrationthe reaction mixture was filtered
  2. washthe filtercake was washed with THF
  3. customThe filtrate was partitioned between water and ethyl acetate
  4. customthe bilayer was separated
  5. extractionthe aqueous portion was extracted twice with ethyl acetate
  6. dry with materialThe combined organic extracts were dried over MgSO4
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated under reduced pressure
  9. customThe resulting residue was purified by flash chromatography (SiO2, ethyl acetate/methanol, 0-10%)
  10. customto afford 0.496 g of (I-5a) as a white solid

出典と根拠

ORDレコード
ord-de9c945bba6446f69dc10414e6b1e3db
出典データセット
uspto-grants-2011_07
特許番号
US07977367B2

反応ノート

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