6-Methyl-2-pyridylmethanol → HCID 70051254, 화합물

HRID 52838

반응식

HRID 52838 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 70051254HCID 70051254, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-283d8e917d9a4c03a44e8ad967461067
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616714

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