Ammonium Hydroxide → HCID 611101, compound

Participants

Reaction Steps

Compound 26 (8.6 mg,0.017 mmol) was dissolved in concentrated NH4OH (0.4 mL) and stirred overnight. The crude product was extracted into CHCl3, and the organic layer was evaporated to dryness. The remaining residue was recrystallized from chloroform/petroleum ether to yield 7.2 mg of 27 (97%); mp 188°-190 ° C.: 1H NMR (CDCl3) δ 2.00-2.70 (m, 12 H), 3.20 (d, J=14 Hz, 1 H), 3.60 (br d, J=14 Hz, 1 H), 7.26 (dd, J= 7.8, 4.7 Hz, 1 H), 7.40 (m, 1 H), 7.55 (dd, J= 7.9, 1.4 Hz, 1 H), 7.58-7.62 (br s, 1 H), 7.92 (d, J= 7.7 Hz, 1 H), 8.26 (br s, 1 H), 9.35 (br s, 1 H); MS (CI/NH3) m/e 381 (MH+base) , 338, 252, 212.

Provenance & Evidence