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Hydrochloric Acid → (E)-N-(4-(2-(dimethylamino)ethoxy)phenyl)-2-(4-hydroxyphenyl)-3-phenylpent-2-enamide

HRID 884054
ノート
印刷プレビュー

反応式

HRID 884054 の反応式
[CH3:1][N:2]([CH3:35])[CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:34])/[C:14](/[C:24]2[CH:29]=[CH:28][C:27]([O:30]COC)=[CH:26][CH:25]=2)=[C:15](/[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)\[CH2:16][CH3:17])=[CH:8][CH:7]=1.Cl.C([O-])(O)=O.[Na+]>CO.O1CCOCC1.O>[CH3:35][N:2]([CH3:1])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([NH:12][C:13](=[O:34])/[C:14](/[C:24]2[CH:29]=[CH:28][C:27]([OH:30])=[CH:26][CH:25]=2)=[C:15](/[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)\[CH2:16][CH3:17])=[CH:10][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 57693048(E)-N-(4-(2-(dimethylamino)ethoxy)phenyl)-2-(4-(methoxymethoxy)phenyl)-3-phenylpent-2-enamide

生成物 1

HCID 11373794(E)-N-(4-(2-(dimethylamino)ethoxy)phenyl)-2-(4-hydroxyphenyl)-3-phenylpent-2-enamide収率 89%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 4 (2.89 g, 6.09 mmol) in MeOH (40 ml) was added 4N HCl in 1,4-dioxane (15.2 ml) under ice cooling, and the mixture was stirred at room temperature for 2 h. A solution of NaHCO3 in H2O was poured into the reaction mixture under ice cooling, and the whole was extracted with AcOEt. The organic layer was washed with brine, dried over Na2SO4, and then concentrated. The residual solid was triturated with AcOEt to give 5 (89%).

後処理

  1. extractionthe whole was extracted with AcOEt
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customThe residual solid was triturated with AcOEt

出典と根拠

ORDレコード
ord-6f17efa535bd4f85a1cdc6a68ec4daaa
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08236987B2

反応ノート

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