Glycine methyl ester hydrochloride → HCID 19801611、化合物

HRID 1646173ノート

反応式

HRID 1646173 の反応式
[CH2:1]([O:3][P:4]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16]Br)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].Cl.[CH3:19][O:20][C:21](=[O:24])[CH2:22][NH2:23]>CO.C(N(CC)CC)C>[CH2:1]([O:3][P:4]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][NH:23][CH2:22][C:21]([O:20][CH3:19])=[O:24])([O:5][CH2:6][CH3:7])=[O:8])[CH3:2]

参加物

5

反応物 2

HCID 122755Glycine methyl ester hydrochlorideHCID 151719952-(Diethylphosphonomethyl)benzyl bromide

生成物 1

HCID 19801611HCID 19801611、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8471Triethylamine溶媒

実験手順

A solution of the diethyl[[2(bromomethyl)phenyl]methyl]phosphonate (Example A) (0.9 g, 2.8 mmol) in methanol (25 ml) and triethylamine (5 ml) is treated with glycine methyl ester hydrochloride (0.71 g, 5.6 mmol) and heated at reflux in an oil bath for 19 hours. The solvent is removed in vacuo and the residue dissolved in water and extracted with chloroform. The chloroform layer is dried over magnesium sulfate, filtered, and evaporated. The oily residue is purified via silica gel chromatography (2-4% methanol in chloroform as eluant).

後処理

  1. temperatureheated
  2. temperatureat reflux in an oil bath for 19 hours
  3. customThe solvent is removed in vacuo
  4. dissolutionthe residue dissolved in water
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform layer is dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe oily residue is purified via silica gel chromatography (2-4% methanol in chloroform as eluant)

出典と根拠

ORDレコード
ord-3c3a607969fc4b34b0b7fac8a867652d
出典データセット
uspto-grants-1993_01
特許番号
US05179085

反応ノート

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