HCID 86674072, compound → HCID 71060167, compound

Participants

Reaction Steps

Compound 5 (167 mg, 0.38 mmol) was incubated in concentrated ammonium hydroxide (4.0 ml) for 1.0 hr at 50 degrees C. The resulting solution was evaporated to dryness and the residue was precipitated from methanol-diethyl ether: 96-mg (74% yield). TLC (50/48/2, ethyl acetate/methanol/acetic acid), Rf=0.50; 1H NMR (DMSO-d6) δ 7.78 (1H, m, aromatic-H), 7.43 (2H, m, aromatic-Hs), 7.18 (1H, m, aromatic-H), 6.95 and 6.26 (2H, 2×s, aromatic-Hs), 2.37 (2H, t, J=6.6 Hz, methylene-Hs), 1.68 (2H, m, methylene-Hs). Note—An additional methylene peak (2Hs) is expected to be hidden under the large water peak covering the range 3.8-3.1 ppm.

Provenance & Evidence