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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethanethiol → HCID 178477296, 화합물

HRID 1633423
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HRID 1633423 반응식
[CH3:1][N:2]=[C:3]([OH:19])[C:4]1[C:5](=[C:9]([N+]([O-])=O)[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7].[CH2:20]([SH:22])[CH3:21].C([O-])(=O)C.[Na+]>C(OCC)(=O)C>[CH3:1][N:2]=[C:3]([OH:19])[C:4]1[C:5](=[C:9]([S:22][CH2:20][CH3:21])[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6343EthanethiolHCID 517045Sodium AcetateHCID 178485491HCID 178485491, 화합물

생성물 1

HCID 178477296HCID 178477296, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

5.02 g (20 mmols) of 3,5-dinitrophthalic acid N-methylimide, 2.73 g (44 mmols) of ethylmercaptan, 8.2 g (1 0 mmols) of anhydrous sodium acetate and 50 ml of ethyl acetate are kept at 25° C. overnight and then kept under reflux, again overnight. The reaction mixture is evaporated, the residue is taken up in methylene chloride/water, the extracts are washed with saturated NaHCO3 solution, dried over sodium sulfate and evaporated and the residue is chromatographed with methylene chloride over 20 g of silica gel. After recrystallisation from methylene chloride/n-pentane, 2.40 g (45% of theory) of 3-ethylthio-5-nitrophthalic acid N-methylimide, with a melting point of 193°-4° C., are obtained.

후처리

  1. temperatureunder reflux, again overnight
  2. customThe reaction mixture is evaporated
  3. washthe extracts are washed with saturated NaHCO3 solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customthe residue is chromatographed with methylene chloride over 20 g of silica gel
  7. customAfter recrystallisation from methylene chloride/n-pentane, 2.40 g (45% of theory) of 3-ethylthio-5-nitrophthalic acid N-methylimide
  8. customwith a melting point of 193°-4° C., are obtained

출처 및 근거

ORD 기록
ord-55661acaf59b4bdd914b876877a43d07
출처 데이터셋
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04480105

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