Hydrochloric Acid → 322394-70-7

Sodium hydride (1.8 g) is added to a solution of N-(diphenylmethylene)glycine ethyl ester in tetrahydrofuran under ice cooling, then the temperature is raised to room temperature, and the mixture is stirred for one hour. 2-Bromoethyl methyl ether (4.22 ml) is added to the mixture, and the whole is refluxed overnight. The reaction mixture is cooled to room temperature, 0.1 N hydrochloric acid is added thereto, and the whole is stirred for four hours. Ethyl acetate is added to the reaction mixture, and the whole is extracted with 0.1 N hydrochloric acid. The extract is basified with a saturated aqueous sodium hydrogencarbonate solution, and the whole is extracted with ethyl acetate. The extract is washed with saturated brine and dried over anhydrous magnesium sulfate. The extract is concentrated under reduced pressure, a 4 N hydrogen chloride/ethyl acetate solution is added to the resulting residue, and the whole is concentrated under reduced pressure again to give the titled reference compound (2.67 g).

1. temperaturethe whole is refluxed overnight
2. temperatureThe reaction mixture is cooled to room temperature
3. stirringthe whole is stirred for four hours
4. extractionthe whole is extracted with 0.1 N hydrochloric acid
5. extractionthe whole is extracted with ethyl acetate
6. washThe extract is washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationThe extract is concentrated under reduced pressure
9. additiona 4 N hydrogen chloride/ethyl acetate solution is added to the resulting residue
10. concentrationthe whole is concentrated under reduced pressure again

ORD record

ord-1264bdd737ce4ff1bc00306a35d44854

Source dataset

uspto-grants-2005_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06960575B2