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Benzoylacetone → HCID 19039879、化合物

HRID 1684572
ノート
印刷プレビュー

反応式

HRID 1684572 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 19039879HCID 19039879、化合物収率 70%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03f9dcf9fe014bb4a1bd18ba671202ca
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05641788

反応ノート

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