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Ethanol → HCID 21709030, 화합물

HRID 651575
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HRID 651575 반응식
O=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[S:5][CH:4]([C:12]([OH:14])=[O:13])[CH2:3]1.[C:15]1([NH:21]N)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.S(=O)(=O)(O)O.[CH2:28](O)[CH3:29]>>[CH:10]1[C:11]2[C:2]3[NH:21][C:15]4[C:20]([C:3]=3[CH:4]([C:12]([O:14][CH2:28][CH3:29])=[O:13])[S:5][C:6]=2[CH:7]=[CH:8][CH:9]=1)=[CH:19][CH:18]=[CH:17][CH:16]=4
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 7516PhenylhydrazineHCID 118391884-Oxothiochromane-2-carboxylic acid

생성물 1

HCID 21709030HCID 21709030, 화합물

실험 절차

To a solution of 22.54 g of (4-oxo-thiochroman-2-yl)carboxylic acid and 10.7 ml of phenylhydrazine in 100 ml of ethanol was added 15 ml of sulfuric acid, followed by reflux under heating for 5 hours. The reaction solution was cooled to room temperature, poured into 500 ml of ice water and extracted with ether. The extract was washed with a saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from ethanol-hexane to give 21.85 g of ethyl 6,11-dihydro-5-thia-11-aza-benzo[a]fluoren-6-carboxylate.

후처리

  1. temperatureby reflux
  2. temperatureunder heating for 5 hours
  3. extractionextracted with ether
  4. washThe extract was washed with a saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. customAfter removal of the drying agent
  7. filtrationby filtration
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customthe residue was recrystallized from ethanol-hexane

출처 및 근거

ORD 기록
ord-cf505bc4bbee4060bf3402fff5e23143
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06281355B1

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