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Ethanol → HCID 9846356, 화합물

HRID 1938342
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HRID 1938342 반응식
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:24]=[C:23]2[C:18]([CH:19]=[C:20]([CH2:25][CH:26]3[S:30][C:29](=N)[NH:28][C:27]3=[O:32])[CH:21]=[N:22]2)=[CH:17][CH:16]=1.C([OH:35])C>Cl>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:24]=[C:23]2[C:18]([CH:19]=[C:20]([CH2:25][CH:26]3[S:30][C:29](=[O:35])[NH:28][C:27]3=[O:32])[CH:21]=[N:22]2)=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 702EthanolHCID 140385021HCID 140385021, 화합물

생성물 1

HCID 9846356HCID 9846356, 화합물수율 11%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

In a mixture of 3N hydrochloric acid (4 mL) and ethanol (2 mL) was dissolved 5-[[7-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-quinolyl]methyl]-2-iminothiazolidin-4-one (100 mg, 0.22 mmol.). The resulting solution was heated under reflux for 12 hours. After the completion of reaction was confirmed, ethanol was distilled off. To the residue were added ethyl acetate and aqueous sodium hydrogen carbonate. The organic portion was recovered, washed with water, and dried over sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/3), to give 11 mg of the desired compound as pale brown crystalline powder (yield 11%).

후처리

  1. temperatureThe resulting solution was heated
  2. temperatureunder reflux for 12 hours
  3. customAfter the completion of reaction
  4. distillationethanol was distilled off
  5. additionTo the residue were added ethyl acetate and aqueous sodium hydrogen carbonate
  6. customThe organic portion was recovered
  7. washwashed with water
  8. dry with materialdried over sodium sulfate
  9. distillationThe solvent was distilled off under reduced pressure
  10. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/3)

출처 및 근거

ORD 기록
ord-0ad267cc8b2c4946926d83cb1dd63dda
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05693651

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