Hydrochloric Acid → HCID 178516734, compound

Temperature

-30 °C

11.05 g (0.1 mol) of glycinamide hydrochloride was dissolved in 200 ml of methanol. To the resultant solution was added a solution of 13.44 g (0.12 mol) of cyclohexane-1,2-dione in 30 ml of methanol under cooling to -30° C. or lower and then, 20 ml of an aqueous 12.5 N NaOH solution was dropwise added thereto. Subsequently, the resultant mixture was stirred at -30° C. or lower for 30 minutes and further stirred at room temperature for 3 hours to effect a reaction. To the resultant reaction mixture was added 25 ml of concentrated hydrochloric acid, followed by stirring for 10 minutes and then, 15 g of sodium hydrogencarbonate was added thereto. The solvent of the reaction mixture was distilled off in vacuo to thereby obtain a residue. Water was added-to the obtained residue, followed by extraction with chloroform three times to obtain an extract. The extract was dried over anhydrous magnesium sulfate and concentrated in vacuo. The resultant residue was recrystallized from acetone, to thereby obtain 9.36 g of 2-hydroxy-5,6,7,8-tetrahydroquinoxaline (yield: 62.4%).

1. customa reaction
2. customTo the resultant reaction mixture
3. stirringby stirring for 10 minutes
4. distillationThe solvent of the reaction mixture was distilled off in vacuo
5. customto thereby obtain a residue
6. extractionfollowed by extraction with chloroform three times
7. customto obtain an extract
8. dry with materialThe extract was dried over anhydrous magnesium sulfate
9. concentrationconcentrated in vacuo
10. customThe resultant residue was recrystallized from acetone

ORD record

ord-159e76a3ba3641fcbcf9751f5a429208

Source dataset

uspto-grants-1996_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05578596