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Methanol → Ethyl N-(methoxycarbonyl)glycinate

HRID 2412316
Notes
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Reaction equation

HRID 2412316 reaction equation
Cl.[CH2:2]([O:4][C:5](=[O:8])[CH2:6][NH2:7])[CH3:3].[CH3:9][OH:10].[N-]=[C:12]=[O:13]>O1CCCC1>[CH2:2]([O:4][C:5](=[O:8])[CH2:6][NH:7][C:9]([O:13][CH3:12])=[O:10])[CH3:3]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 887MethanolHCID 105034IsocyanateHCID 2723640Glycine ethyl ester, hydrochloride

Product 1

HCID 235150Ethyl N-(methoxycarbonyl)glycinate

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Alternatively, glycine ethyl ester hydrochloride (40.1 g, 0.28 mole) suspended in dry tetrahydrofuran (200 ml) and phosgene were bubbled through the reaction mixture for 0.5 hrs, as the reaction mixture was refluxed. At the end of 0.5 hrs., the reaction was cooled to room temperature and toluene was added followed by the distillation of THF. The reaction mixture containing toluene was further refluxed for 1 hr. The unreacted glycine ethyl ester hydrochloride was filtered and the filtrate containing glycine ethyl ester isocyanate (IR 2250 cm-1) was reacted with excess (2-3 mole) anhydrous methanol and, when the isocyanate peak disappeared, the solvent was removed to isolate N-carbomethoxyglycine ethyl ester.

Workup

  1. customphosgene were bubbled through the reaction mixture for 0.5 hrs, as the reaction mixture
  2. temperaturewas refluxed
  3. customAt the end of 0.5 hrs
  4. additiontoluene was added
  5. distillationfollowed by the distillation of THF
  6. additionThe reaction mixture containing toluene
  7. temperaturewas further refluxed for 1 hr
  8. filtrationThe unreacted glycine ethyl ester hydrochloride was filtered
  9. additionthe filtrate containing glycine ethyl ester isocyanate (IR 2250 cm-1)
  10. customthe solvent was removed

Sources & evidence

ORD record
ord-c2e26164a4814f2490e474bd28d0bc9a
Source dataset
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04491548

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes