Trifluoroacetic acid → HCID 9925055, compound

Participants

Reaction Steps

The product of STEP 8 (370 mg, 0.95 mmol) was dissolved in 20 ml methanol and 20 ml 1N sodium hydroxide solution . The reaction was stirred at room temperature for 16 h, and acidified with trifluoroacetic acid (3 ml). Solvents were evaporated and residue was purified on HPLC using acetonitrile gradient 10-50% in 30 min to yield 300 mg. FAB-MS: (MH+)=361. H NMR(CDCl3) δ1.03 (s, 6H), 2.20 (s, 2H), 2.22 (p, 2H), 2.62 (s, 2IH), 3.58 (q, 2H), 4.14 (t, 2H), 6.72 (t, 1H), 6.86-6.98 (m, 4H), 7.70 (m, 2H); Anal. Calcd. for C20H25N2O3F plus 1.4 CF3COOH: C, 52.66; H, 5.12; N, 5.39. Found: C, 52.56; H, 5.23; N, 5.09.

Provenance & Evidence