4-nitrobutyramide synthesis

Yield:15473-27-5 78%

Reaction Conditions:

with ammonia in methanol at 0 - 20; for 72 h;

Steps:

1 4-Nitro-Butyramide

To a solution of methyl 4-nitrobutyrate (8.83 g, 60 mmol) in methanol (20 mL) at 0° C. was added a solution of ammonia in methanol (7N, 30 mL). The solution was then warmed to room temperature and stirred at for 72 h. The solvent was evaporated and the residue was re-crystallized from ethyl acetate to give the title product (6.2 g, 78%). ¹H NMR (acetone-d₆): 6.86 (bs, NH, 1H), 6.28 (bs, NH, 1H), 4.59 (t, J=6.9 Hz, 2H), 2.36-2.30 (m, 2H), 2.28-2.20 (m, 2H).

References:

US2008/300191,2008,A1 Location in patent:Page/Page column 15