Ethanol → HCID 86720744, compound

To an ethanol (10 mL) suspension of tert-butyl N-methylglycinate hydrochloride (3.0 g), under ice cooling, triethylamine (2.3 mL) was added, and the resultant was stirred at room temperature for 20 minutes. Then, ethyl formate (2.7 ml) was added thereto, and the resultant was stirred at 70° C. for 1 hour. After standing to cool to room temperature and stirring for 4 hours, the reaction solution was concentrated under reduced pressure. The obtained residue was dissolved by the addition of water and a 10:1 chloroform/methanol solution. An organic layer was separated, and an aqueous layer was subjected to extraction with a 10:1 chloroform/methanol solution. The organic layers were dried over magnesium sulfate, and the desiccant was filtered off. Then, the solvent was distilled off under reduced pressure to obtain the title compound (1.9 g) as a light brown oil.

1. stirringthe resultant was stirred at 70° C. for 1 hour
2. temperatureto cool to room temperature
3. stirringstirring for 4 hours
4. concentrationthe reaction solution was concentrated under reduced pressure
5. dissolutionThe obtained residue was dissolved by the addition of water
6. customAn organic layer was separated
7. extractionan aqueous layer was subjected to extraction with a 10:1 chloroform/methanol solution
8. dry with materialThe organic layers were dried over magnesium sulfate
9. filtrationthe desiccant was filtered off
10. distillationThen, the solvent was distilled off under reduced pressure

ORD record

ord-79a1717e6436402ba62c5cf378789048

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09045466B2