HCID 86659601, compound → HCID 58529808, compound

Participants

Reaction Conditions

Reaction Steps

The product from step 2 (20.25 g, 43.68 mmol) was dissolved in 125 mL of AcOH and stirred at 40° C. for 8 h and then concentrated in vacuo. The residue was dissolved in EtOAc (200 mL) and extracted with 50 mL of water, 2×100 mL 2M aq. Na2CO3, brine, dried over Na2SO2. The mixture was filtered through a 1″×4″ pad of SiO2 (pre-wetted with EtOAc) and the pad was washed with 300 mL of EtOAc and the filtrate concentrated in vacuo to give the title compounds as a light, brown syrup that was used without further purification. 1H NMR (300 MHz, DMSO-d6) δ 10.14 (bs, 1H), 7.40-7.24 (m, 5H), 6.59 (d, 1H), 5.90 (dd, 1H), 5.78 (d, 1H), 5.15-4.92 (m, 2H), 4.13 (bd, 1H), 3.99 (bd, 1H), 2.91-2.60 (m, 3H), 1.91 (m, 1H), 1.74-1.62, (m, 1H), 1.42 (s, 12H). ES-MS m/z 400.0 [M+H]+, HPLC RT (min) 3.93

Provenance & Evidence