Triethylamine → HCID 18706304、化合物

HRID 1422211ノート

反応式

HRID 1422211 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16]Br)[CH:3]=1.C(N(CC)CC)C.Cl.[C:26]([O:30][C:31](=[O:34])[CH2:32][NH2:33])([CH3:29])([CH3:28])[CH3:27]>C(#N)C>[C:26]([O:30][C:31](=[O:34])[CH2:32][NH:33][CH2:16][C:4]1[CH:3]=[C:2]([Br:1])[CH:11]=[C:10]2[C:5]=1[N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)([CH3:29])([CH3:28])[CH3:27]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2725036Glycine tert-butyl ester hydrochlorideHCID 23298010HCID 23298010、化合物

生成物 1

HCID 18706304HCID 18706304、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

850 mg (2.35 mmol) of 7-bromo-5-bromomethyl-2,3-dimethoxy-quinoxaline, 0.982 ml of triethylamine and 719 mg of glycine tert-butyl ester hydrochloride are dissolved in 15 ml of acetonitrile and the solution is stirred at reflux for 18 hours. The mixture is concentrated by evaporation and the residue is dissolved in diethyl ether and washed with aqueous 5% sodium carbonate solution and brine. The organic phases are combined, dried over magnesium sulfate and concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate and petroleum ether (1:2). The title compound is obtained in the form of a yellow oil.

後処理

  1. temperatureat reflux for 18 hours
  2. concentrationThe mixture is concentrated by evaporation
  3. dissolutionthe residue is dissolved in diethyl ether
  4. washwashed with aqueous 5% sodium carbonate solution and brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated by evaporation
  7. customThe residue is chromatographed on silica gel with ethyl acetate and petroleum ether (1:2)

出典と根拠

ORDレコード
ord-c594df89354644afb155b893db9dca5c
出典データセット
uspto-grants-2000_06
特許番号
US06080743

反応ノート

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