Acetic Acid → HCID 18314476, 화합물

HRID 1274591노트

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HRID 1274591 반응식
[CH3:1][C:2]([CH3:20])([C:8]1[C:12]2[CH:13]=[C:14]([N+:17]([O-])=O)[CH:15]=[CH:16][C:11]=2[S:10][N:9]=1)[C:3]([O:5][CH2:6][CH3:7])=[O:4].C(O)(=O)C.C(OCC)(=O)C.C(=O)([O-])O.[Na+]>C(Cl)Cl.[Fe]>[NH2:17][C:14]1[CH:15]=[CH:16][C:11]2[S:10][N:9]=[C:8]([C:2]([CH3:20])([CH3:1])[C:3]([O:5][CH2:6][CH3:7])=[O:4])[C:12]=2[CH:13]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8857Ethyl Acetate2회HCID 516892Sodium BicarbonateHCID 18314471HCID 18314471, 화합물

생성물 1

HCID 18314476HCID 18314476, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 6344Dichloromethane용매

반응 조건

온도
56 °C

실험 절차

A mixture of ethyl α,α-dimethyl-5-nitro-1,2-benzisothiazole-3-acetate (0.714 g, 2.42 mmol), iron powder (0.500 g), 10% acetic acid (23.0 mL) and ethyl acetate (23.0 mL) is stirred at 54-58° C. for one hour, cooled, and poured into saturated sodium hydrogen carbonate solution. The resultant aqueous mixture is extracted with ethyl acetate. The combined organic extracts are washed sequentially with water and brine, dried over anhydrous sodium sulfate, and concentrated in vacuo to obtain a yellow oil. Column chromatography of the oil using silica gel and a 10% ethyl acetate in methylene chloride solution gives the title product as a light brown oil which is identified by NMR spectral analysis.

후처리

  1. temperaturecooled
  2. extractionThe resultant aqueous mixture is extracted with ethyl acetate
  3. washThe combined organic extracts are washed sequentially with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto obtain a yellow oil

출처 및 근거

ORD 기록
ord-05df56dcc04a461fbd5d54bf68ea1576
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06156700

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