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Water → HCID 22321558, 화합물

HRID 496551
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HRID 496551 반응식
[N+](=[CH:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][N:7]=1)=[O:5])=[N-].FC(F)(F)C(O)=[O:15].O>C(OCC)C>[OH:15][CH2:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][N:7]=1)=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 73882386HCID 73882386, 화합물

생성물 1

HCID 22321558HCID 22321558, 화합물수율 61%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

2-Diazo-1-(5-methylisoxazol-3-yl)ethanone (7.0 g, 46 mmol) was dissolved in diethyl ether (100 ml) and trifluoroacetic acid (25 ml) and water (100 ml) were added. The solution was stirred at room temperature for 2 hours, then the diethyl ether was removed in vacuo and the aqueous solution was stirred at room temperature for 18 hours. Further water (100 ml) was added and the aqueous solution was extracted twice with ethyl acetate. The organic extracts were washed successively with water, 10% aqueous potassium carbonate solution and brine, and dried (Na2SO4). Evaporation of the solvent yielded the title-compound as a pale solid (4.0 g, 61%), 1H NMR (360 MHz, CDCl3) 2.52 (3H, s), 4.90 (2H, s), 6.44 (1H, s).

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후처리

  1. customthe diethyl ether was removed in vacuo
  2. stirringthe aqueous solution was stirred at room temperature for 18 hours
  3. additionFurther water (100 ml) was added
  4. extractionthe aqueous solution was extracted twice with ethyl acetate
  5. washThe organic extracts were washed successively with water, 10% aqueous potassium carbonate solution and brine
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-d342fd922f664990a433ca57590d5266
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06946461B2

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