Tetrahydrofuran → HCID 178504852, 화합물

HRID 1011495노트

반응식

HRID 1011495 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178504852HCID 178504852, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-de9c945bba6446f69dc10414e6b1e3db
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977367B2

반응 노트

불러오는 중…