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HCID 69960253、化合物 → HCID 18919039、化合物

HRID 1291405
ノート
印刷プレビュー

反応式

HRID 1291405 の反応式
C([O:4][C:5]1[CH:33]=[CH:32][C:8]([C:9]([C:11]2[CH:16]=[CH:15][C:14]([CH:17]=[CH:18][C:19]3[N:28]([CH3:29])[C:27](=[O:30])[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][C:25]=4[CH3:31])[N:20]=3)=[CH:13][CH:12]=2)=[O:10])=[CH:7][CH:6]=1)(=O)C>C1COCC1.C(OCC)(=O)C.CO.[Pd]>[CH3:29][N:28]1[C:27](=[O:30])[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][C:25]=2[CH3:31])[N:20]=[C:19]1[CH2:18][CH2:17][C:14]1[CH:15]=[CH:16][C:11]([C:9](=[O:10])[C:8]2[CH:7]=[CH:6][C:5]([OH:4])=[CH:33][CH:32]=2)=[CH:12][CH:13]=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 1

HCID 69960253HCID 69960253、化合物

生成物 1

HCID 18919039HCID 18919039、化合物収率 93.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 19895526THF ethyl acetate methanol溶媒

実験手順

To a solution of 2-[2-[4-(4-acetoxybenzoyl)phenyl]vinyl]-3,5-dimethyl-4(3H)-quinazolinone (631 mg) in THF-ethyl acetate-methanol (1:1:1) (50 ml) was added 10% Pd/C (50% hydrous) (126 mg) and the mixture was stirred under hydrogen at room temperature for 2 hours. The catalyst was then filtered off and the filtrate was concentrated. After the residue was suspended in ethanol (10 ml), 1N-aqueous sodium hydroxide solution (2.9 ml) was added and the mixture was stirred at room temperature for 2 hours. This reaction mixture was concentrated and the residue was suspended in water (20 ml) and neutralized with 1N-hydrochloric acid (2.9 ml). The precipitate was collected by filtration, washed with water, and dried to provide 538 mg of white powder.

後処理

  1. filtrationThe catalyst was then filtered off
  2. concentrationthe filtrate was concentrated
  3. addition1N-aqueous sodium hydroxide solution (2.9 ml) was added
  4. stirringthe mixture was stirred at room temperature for 2 hours
  5. concentrationThis reaction mixture was concentrated
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-62f49d39a85b48f1aecc12a5a26a74d8
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753664

反応ノート

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