HCID 616538, compound → 4-methyl-7-Amino-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

Participants

Reaction Steps

Intermediate 1 (3.48 g, 15 mmol, preparation described in Example 1) was suspended in a 120 mL of 1:1 solution of THF/Ethanol. The suspension was treated with nitrogen followed by vacuum, before adding Pd/C 10% (0.7 g), suspended in ethanol. The reaction vessel was then fitted onto the Parr hydrogenator and left under hydrogen pressure (20 psi) for about 3 hours with stirring. The excess hydrogen gas was removed using vacuum and then nitrogen was purged through the solution. The catalyst was filtered off using celite and the filtrate was evaporated to the minimum amount of ethanol. A white precipitate formed which was separated by filtration and dried under vacuum to afford 918 mg of desired material 3 in 30% yield.

Provenance & Evidence