Hydrochloric Acid → Methyl 4-aminooxane-4-carboxylate

A solution 4-aminotetrahydro-2H-pyran-4-carboxylic acid (0.50 g, 3.4 mmol) in MeOH (10 mL) was saturated with HCl gas at 0-5° C., and the mixture was then heated at reflux for 3.5 h. The solvents were evaporated in vacuo, the residue was dissolved in saturated aqueous NaHCO3 and the aqueous solution was extracted with CH2Cl2 (2×50 mL). The combined extracts were dried (MgSO4) and evaporated in vacuo to give methyl 4-aminotetrahydro-2H-pyran-4-carboxylate (410 mg, 2.58 mmol).

1. temperaturethe mixture was then heated
2. temperatureat reflux for 3.5 h
3. customThe solvents were evaporated in vacuo
4. dissolutionthe residue was dissolved in saturated aqueous NaHCO3
5. extractionthe aqueous solution was extracted with CH2Cl2 (2×50 mL)
6. dry with materialThe combined extracts were dried (MgSO4)
7. customevaporated in vacuo

ORD-Eintrag

ord-e19565faaf4b4107b4d5d0f5c62c2d9b

Quelldatensatz

uspto-grants-2000_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06093731