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Lithium hydroxide, monohydrate → (E)-N-indan-1-yl-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acrylamide

HRID 1362591
ノート
印刷プレビュー

反応式

HRID 1362591 の反応式
O.[OH-].[Li+].[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[N:14]1[CH:18]=[C:17]([CH3:19])[N:16]=[CH:15]1)[CH:9]=O.C(OP([CH2:28][C:29](=[O:40])[NH:30][CH:31]1[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=2)[CH2:33][CH2:32]1)(=O)OCC)C>C1COCC1>[CH:31]1([NH:30][C:29](=[O:40])/[CH:28]=[CH:9]/[C:8]2[CH:11]=[CH:12][C:13]([N:14]3[CH:18]=[C:17]([CH3:19])[N:16]=[CH:15]3)=[C:6]([O:5][CH3:4])[CH:7]=2)[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=2)[CH2:33][CH2:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 168937Lithium hydroxide, monohydrateHCID 272824453-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzaldehydeHCID 86602465(Indan-1-ylcarbamoylmethyl)phosphonic acid diethyl ester

生成物 1

HCID 59170837(E)-N-indan-1-yl-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acrylamide収率 36.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

Lithium hydroxide monohydrate (9 mg) was added to a THF (2 mL) solution of 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzaldehyde (21 mg) and indan-1-ylcarbamoylmethylphosphonic acid diethyl ester (30 mg) obtained above, and the reaction solution was agitated at room temperature overnight. After the reaction mixture was concentrated under reduced pressure, the residue was purified by silica gel column chromatography (Carrier: Chromatorex™ NH, elution solvent: hexane-ethyl acetate system), and 13 mg of the title compound was obtained.

後処理

  1. customobtained above, and the reaction solution
  2. concentrationAfter the reaction mixture was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (Carrier: Chromatorex™ NH, elution solvent: hexane-ethyl acetate system)

出典と根拠

ORDレコード
ord-03f93050bfc24be591306470faa2ea65
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07880009B2

反応ノート

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