6-Methyl-2-pyridylmethanol → HCID 70051254、化合物

HRID 52838

反応式

HRID 52838 の反応式
[N-:1]=[C:2]=[O:3].[CH3:4][O:5][C:6](=[O:12])[C@H:7]([CH:9]([CH3:11])[CH3:10])N.[CH3:13][C:14]1[N:19]=[C:18]([CH2:20][OH:21])[CH:17]=[CH:16][CH:15]=1>C1(C)C=CC=CC=1>[CH3:4][O:5][C:6](=[O:12])[C@H:7]([CH:9]([CH3:11])[CH3:10])[NH:1][C:2]([O:21][CH2:20][C:18]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:13])[N:19]=1)=[O:3]

参加物

5

反応物 3

HCID 707366-Methyl-2-pyridylmethanolHCID 94285Valine methyl esterHCID 105034Isocyanate

生成物 1

HCID 70051254HCID 70051254、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of the isocyanate derived from Valine methyl ester (17.9 mmol) dissolved in toluene was added 6-methyl-pyridine-2-methanol (2.42 g, 1.1 equivalent). The solution was he ated at reflux for 2 hours. After concentration in vacuo and purifiction by silica gel column chromatography, (6-methylpyridin-2-yl)methoxycarbonyl-Valine methyl ester (2.8 g) was obtained. Hydrolysis of the methyl ester using aqueous lithium hydroxide provide the title compound upon recrystallization from hot ethyl acetate.

後処理

  1. temperatureat reflux for 2 hours
  2. concentrationAfter concentration in vacuo and purifiction by silica gel column chromatography

出典と根拠

ORDレコード
ord-283d8e917d9a4c03a44e8ad967461067
出典データセット
uspto-grants-1997_04
特許番号
US05616714

関連ノート

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