(3,4-Dinitrophenyl)(morpholino)methanone → 4-(3,4-Dinitrobenzyl)morpholine

Participants

Reaction Steps

4-(3,4-Dinitro-benzyl)-niorpholme (2.815 kg, 10.53 mol, 1.O wt) and methanol (12.00 L, 4.3 vol) were charged to a flask under nitrogen and heated to 65 to 7O° C. The temperature was maintained until complete dissolution. The mixture was then cooled to and aged at 0 to 5° C. for 1 hour. The solids were isolated by filtration. The filter-cake was washed with methanol (2×1.50 L, 2×0.5 vol) and dried under vacuum at 35 to 45° C. to give 4-(3,4-dinitro-benzyl)-morpholine (2.353 Kg, 83.5% based on input Stage 2, 82.5% overall yield based on total input Stage 1 material) as a yellow solid.

Provenance & Evidence