Trifluoroacetic acid → HCID 12018741, compound

Participants

Reaction Steps

The product of STEP 9 (148 mg, 0.35 mmol) was dissolved in 5 ml methanol and 5 ml 1N sodium hydroxide solution. The reaction was stirred at room temperature for 18 h, acidified with 2 ml trifluoroacetic acid, and concentrated. The residue was purified on HPLC using acetonitrile gradient 10-50% in 30 min to yield 90.6 mg. FAB-MS:(MH+)=406.5. H NMR (DMSO-d6) δ1.43 (s, 3H), 2.03 (p, 2H), 2.61 (d, 1H), 2.92 (d,1IH), 2.96 (d, 1H), 3.07 (d, 1H), 3.48 (t, 2H), 4.01 (t, 2H), 6.76 (s, 4H), 6.85 (t,1H), 7.06 (d, 1H), 7.88 (m, 2H), 7.93 (d, 1H), 8.40 (d, 1H), 8.72 (d,1H), 8.76 (s, 1H), 8.90 (br, 1H); Anal Calcd. for C24H27N3O3 plus 2.75 CF3COOH: C, 48.67; H, 4.26; N, 5.77. Found: 48.56; H, 4.29; N, 6.05.

Provenance & Evidence