Methanol → 2-Chloro-5-(methylsulphonyl)benzoic acid

HRID 375890노트

반응식

HRID 375890 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:8](SC)=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].O[O:14][S:15]([O-:17])=O.[K+].[CH3:19]O>O>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:15]([CH3:19])(=[O:17])=[O:14])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

5

반응물 3

HCID 887MethanolHCID 6088142-Chloro-5-(methylsulfanyl)benzoic acidHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 23291322-Chloro-5-(methylsulphonyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A solution of 2-chloro-5-(methylthio)benzoic acid (25 g, 123 mmol) dissolved in methanol (500 ml) was cooled to 0°-5° C. and then OXONE® (227.6 g, 370 mol) in water (500 ml) was added. The reaction mixture was stirred for 30 minutes at 0°-5° C. and then at room temperature for 4 hours. The reaction mixture was diluted with water, extracted with CHCl3 (3×200 ml) and the CHCl3 extracts were combined, washed with water, then brine and then were dried over MgSO4, filtered and evaporated to afford 5.13 g of 2-chloro-5-(methylsulfonyl)benzoic acid, m.p. 187°-188° C.

후처리

  1. temperaturewas cooled to 0°-5° C.
  2. waitat room temperature for 4 hours
  3. extractionextracted with CHCl3 (3×200 ml)
  4. washwashed with water
  5. dry with materialbrine and then were dried over MgSO4
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-95597c707e3f4cba9c2fd1429fd83355
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05488055

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