Glycine methyl ester hydrochloride → HCID 19801611, 화합물

HRID 1646173노트

반응식

HRID 1646173 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 19801611HCID 19801611, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8471Triethylamine용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-3c3a607969fc4b34b0b7fac8a867652d
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05179085

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