1,2,4,5-BENZENETETRAMINE TETRAHYDROCHLORIDE synthesis

Yield:4506-66-5 81%

Reaction Conditions:

Stage #1: 1,3-diamino-4,6-dinitrobenzenewith tin;Degussa F₁₀₁ catalyst;hydrogen in ethanol at 80.5; under 15514.9 Torr; for 2 h;Autoclave;Inert atmosphere;
Stage #2: with hydrogenchloride in ethanol;lithium hydroxide monohydrate at 15;

Steps:

1,2,4,5-tetraminobenzene tetrahydrochloride

1,2,4,5-tetraminobenzene and its mineral and organic acid salts are susceptible to oxidation and should be handled in an inert atmosphere. To a 2 gallon autoclave was added 480 g of 1,5-diamino-2,4-dinitrobenzene, 5.5 g of Ttin powder, and 9.6 g of Degussa F101 Pt/C catalyst. The clave was then sealed, purged with nitrogen, and had added to it 2000 mL of nitrogen sparged ethanol. The clave was heated to 70° C. and pressurized to 300 psi with hydrogen and then kept at 80.5° C. and 300 psi for 2 h. After 2 h, the claves contents were pushed through a solids filter and into a precipitation vessel where they were cooled to 15° C. and the product precipitated with the addition 1400 mL of 12.1M HCl. The precipitated solids were collected, washed with 12.1 M HCl and ethanol, and partially dried on the filter at 40° C. with nitrogen and vacuum. This afforded 557.3 g (81% yield) of 1,2,4,5-tetraminobenzene tetrahydrochloride.; The 1,2,4,5-tetraminobenzene tetrahydrochloride can be further purified by crystallization from aqueous with concentrated hydrochloric acid.

References:

US2014/66629,2014,A1 Location in patent:Paragraph 0073-0075