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Ethyl Acetate → 7-Hydroxy-2-(4-hydroxy-phenyl)-3-{4-[2-(piperidin-1-yl)-ethoxy]-phenyl}-3H-quinazolin-4-one

HRID 617126
ノート
印刷プレビュー

反応式

HRID 617126 の反応式
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:20](=[O:21])[C:19]3[C:14](=[CH:15][C:16]([OH:22])=[CH:17][CH:18]=3)[N:13]=[C:12]2[C:23]2[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=2)=[CH:7][CH:6]=1.C(O[CH2:34][CH3:35])(=O)C>N1CCCCC1>[OH:22][C:16]1[CH:15]=[C:14]2[C:19]([C:20](=[O:21])[N:11]([C:8]3[CH:9]=[CH:10][C:5]([O:4][CH2:3][CH2:2][N:11]4[CH2:35][CH2:34][CH2:6][CH2:7][CH2:8]4)=[CH:6][CH:7]=3)[C:12]([C:23]3[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=3)=[N:13]2)=[CH:18][CH:17]=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 8857Ethyl AcetateHCID 1358228303-[4-(2-Chloro-ethoxy)-phenyl]-7-hydroxy-2-(4-hydroxy-phenyl)-3H-quinazolin-4-one

生成物 1

HCID 1355441217-Hydroxy-2-(4-hydroxy-phenyl)-3-{4-[2-(piperidin-1-yl)-ethoxy]-phenyl}-3H-quinazolin-4-one

試薬・触媒・溶媒 1

HCID 8082Piperidine溶媒

実験手順

A solution containing 0.25 g (0.000612 mol) of 3-[4-(2-chloro-ethoxy)-phenyl]-7-hydroxy-2-(4-hydroxy-phenyl)-3H-quinazolin-4-one in 7 mL of piperidine was stirred and heated to reflux for 2 hours. After cooling to room temperature, ethyl acetate was added to the reaction mixture and the solvents were co-evaporated to near dryness in a rotary evaporator. The dark residue was extracted with ethyl acetate and water. The aqueous layer was removed and chilled on ice. The precipitate which then formed was collected by vacuum filtration (0.052 g, mp 185-190° C.) and was shown to be the hydrochloride salt monohydrate.

後処理

  1. temperatureheated
  2. temperatureto reflux for 2 hours
  3. customin a rotary evaporator
  4. extractionThe dark residue was extracted with ethyl acetate and water
  5. customThe aqueous layer was removed
  6. temperaturechilled on ice
  7. customThe precipitate which then formed
  8. filtrationwas collected by vacuum filtration (0.052 g, mp 185-190° C.)

出典と根拠

ORDレコード
ord-9eb72418a59d4e4d8468e3a7f6857f09
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05948775

反応ノート

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