Sulfuric Acid → HCID 12852684, compound

Participants

Reaction Conditions

Reaction Steps

3-Cyano-1,2-dihydro-2-oxocyclohepta[b]pyrrole-1-acetic acid ethyl ester (2.56 g, described in example 12), was suspended in concentrated H2SO4 (10 ml). The mixture was stirred at 25° C. for 3 hr and then poured into ice water (20 ml). After 5 minutes, the resulting solid was collected on a filter, washed with water and then diethyl ether, air dried and recrystallized from ethanoldiethyl ether to give 1.75 g of 3-(aminocarbonyl)-1,2-dihydro-2-oxocyclohepta[b]pyrrole-1-acetic acid ethyl ester; mp 215°-220° C.; nmr (DMSO-d6) δ1.20 (t,J=7.5 Hz, 3H), 3.25 (broad, 2H), 4.15 (q, J=7.5 Hz, 2H), 5.0 (s, 2H), 7.6 (m, 4H), 9.3 (d, J=10 Hz, 1H); ir (white mineral oil) 3360, 3160, 1743, 1734, 1667, 1590 cm-1 ; uvλmax (MeOH) 276 nm (ε32,100), 232 (17,200), 223 (17,100); Anal Calc for C14H14N2O4 : C, 61.36% H, 5.15% N, 10.21%; Found: C, 61.12% H, 5.26% N, 10.24%.

Provenance & Evidence