HCID 117664395, compound → HCID 117664725, compound

Participants

Reaction Steps

Dissolve compound 8 (3 g, 0.0085 mol) in 30 ml 20% aqueous sodium hydroxide solution, heat to reflux for 2 h, cool the solution to stop the reaction. Add in 10% dilute hydrochloric acid to adjust the pH to less than 2 to cause a formation of a large amount of white precipitation, filter and dry the precipitation to obtain a white solid, dissolve it in petroleum ethe/ethyl acetate and recrystallize to obtain 2.6 g white solid (90%). 1H-NMR (400M, CDCl3) δ (ppm): 1.61 (s, 3H), 1.71 (s, 3H), 3.24 (d, J=6.8 Hz, 2H), 3.91 (s, 3H), 5.12 (t, J=6.8 Hz, 1H), 6.78 (s, 1H), 7.00 (d, J=16 Hz, 1H), 7.27 (t, J=7.2 Hz, 1H), 7.38 (t, J=7.2 Hz, 2H), 7.52 (d, J=7.2 Hz, 2H), 7.84 (d, J=16 Hz, 1H), 12.28 (s, 1H). ESI-MS mz: 361.14318 [M+Na]+ (Calcd. for C21H22O4Na: 361.14158).

Provenance & Evidence