Methanol → HCID 58721700, compound

Participants

Reaction Conditions

Reaction Steps

1-[9-(4-Chlorophenyl)-8-(2-chlorophenyl)-9H-purin-6-yl]-4-methylaminopiperidine-4-carboxylic acid amide 7A-87 (Example 164; 53 mg, 0.093 mmol) and Amberlyst 15 (0.8 g) in methanol (5 ml) was sealed in a tube and then heated to 60° C. for 20 h. The resin was removed by filtration and washed with 2:1 methanol/triethylamine and then 10% NH4OH in methanol. The combined organic layers were concentrated and then purified on a Biotage™ Flash 12S column using 0–2–4% methanol in methylene chloride as eluant to give title compound 21A-1 as a light brown solid (26 mg, 55%): +ESI MS (M+1) 511.1; 1H NMR (400 MHz, CD2Cl2) δ 8.28 (s, 1H), 7.52 (d, J=8.3 Hz, 1H), 7.44–7.32 (m, 5H), 7.21 (d, J=8.7 Hz, 2H), 5.55 (v br s, 1H), 4.65 (v br s, 2H), 4.13 (v br s, 2H), 3.71 (s, 3H), 2.28 (s, 3H), 2.07 (ddd, J=13.7, 9.6, 3.7 Hz, 2H), 1.79 (dt, J=13.7, 3.9 Hz, 2H).

Provenance & Evidence