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Benzoylacetone → HCID 19039879, 화합물

HRID 1684572
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HRID 1684572 반응식
Cl.[NH2:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[CH:17][C:4]=1[C:5]([C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[C:9]([O:15][CH3:16])[CH:8]=1)=O.[C:25]([CH2:33][C:34](=O)[CH3:35])(=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>C(O)C>[C:25]([C:33]1[C:34]([CH3:35])=[N:2][C:3]2[C:4]([C:5]=1[C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[C:9]([O:15][CH3:16])[CH:8]=1)=[CH:17][C:18]([O:23][CH3:24])=[C:19]([O:21][CH3:22])[CH:20]=2)(=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7166BenzoylacetoneHCID 214661342-Amino-3',4',4,5-tetramethoxybenzophenone hydrochloride

생성물 1

HCID 19039879HCID 19039879, 화합물수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2-amino-4,5,3',4'-tetramethoxy-benzophenone hydrochloride (2.0 g), benzoylacetone (0.917 g) and ethanol (35 ml) was stirred under reflux for 1 hour. The reaction mixture was concentrated under reduced pressure. The residue was poured into a saturated aqueous solution of sodium bicarbonate, and the mixture was extracted with chloroform. The chloroform layer was washed with water, dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-ethyl acetate (10:1, v/v) gave 3-benzoyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxy-2-methylquinoline (1.75 g, 70%). This compound was recrystallized from ethanol to give colorless prisms, mp. 151°-152° C.

후처리

  1. temperatureunder reflux for 1 hour
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionThe residue was poured into a saturated aqueous solution of sodium bicarbonate
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. washThe fractions eluted with chloroform-ethyl acetate (10:1

출처 및 근거

ORD 기록
ord-03f9dcf9fe014bb4a1bd18ba671202ca
출처 데이터셋
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05641788

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