Hydrochloric Acid → HCID 22675496, compound

Stannous chloride dihydrate (22.5 g, 0.1M) was added in one portion to .a stirred mixture of N-ethyl-5-bromo-2-nitrobenzylamine (8.5 g, 32.8 mmol) and 36% hydrochloric acid (20 ml, 0.22M) in ethanol (250 ml) at ambient temperature. There was an exothermic reaction (50° C.) and a yellow solution formed, which was stirred for 1 hour allowing it to cool. The solvent was evaporated at reduced pressure and the residue dissolved in ethanol (100 ml) and stirred while diluting with ether (200 ml) until crystallisation occurred. The yellow solid was filtered off and washed with ether to give N-ethyl-5-bromo-2-aminobenzylamine as a salt, from which the free base was isolated by stirring with 2N sodium hydroxide solution (150 ml) and extracting into ether. The organic layer was dried over anhydrous magnesium sulphate and evaporated to give an oil (4.2 g).

1. customan exothermic reaction (50° C.)
2. customa yellow solution formed
3. stirringwhich was stirred for 1 hour
4. temperatureto cool
5. customThe solvent was evaporated at reduced pressure
6. dissolutionthe residue dissolved in ethanol (100 ml)
7. stirringstirred
8. additionwhile diluting with ether (200 ml) until crystallisation
9. filtrationThe yellow solid was filtered off
10. washwashed with ether

ORD record

ord-75760247e271424bb7d3d18e741aca9d

Source dataset

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05834468