HCID 70431189, compound → HCID 70431208, compound

Participants

Reaction Steps

The O-benzyl derivative (51) (23.08 g) was taken up in THF (250 ml) and hydrogenolysed in the presence of 10% Pd/C until no starting material remained. The solution was filtered through Kieselguhr and the filtrate evaporated to give a white solid (52) (16.63 g), m.p. 94°-96° C. (from EtoAc--hexane), νmax (KBr) 3400, 1795, 1770, 1720, and 1400 cm-1, δ(CDCl3) 1.45(d, J6.5 Hz, 3H) (irradiation at 4.18 caused this signal to collapse to a s), 4.18 (dq, j6.5 and 2 Hz, 1H), 4.70(d, J2 Hz, 1H) (irradiation at 4.18 caused this signal to collapse to a s), 7.3-8.0 (m, 4H), and 7.7-8.7br (1H, exch.), m/e 246(M+) and 187 (base peak). (Found: C, 58.28; H, 4.11; N, 11.46; M+ 246.0647. C12H10N2O4 requires C, 58.54; H, 4.09; N, 11.38%, M, 246.0681).

Provenance & Evidence