反应详情

hydrochloride. To a stirred solution of tert-butyl(3S)-3-({[2-[(aminocarbonyl)amino]-5-(4-methoxyphenyl)-3-thienyl]carbonyl}amino)azepane-1-carboxylate (0.9 g, 1.8 mmol) in 1,4-dioxane (10 mL) was added 4.0N HCl in 1,4-dioxane (10 mL, 40 mmol). A precipitate forms shortly and the reaction is stirred for an additional 4 h at room temperature. Due to the hygroscopic nature of the salt form, the solvent was removed under vacuum. The residue was dissolved in methanol and concentrated under vacuum (2×) to yield and off-white solid. Recrystallization from using 2-propanol gave 0.45 g (59%) of a white solid. 1H NMR (d6-DMSO, δ 10.9, s, 1H; δ 9.58, br s, 1H; δ 9.29, br s, 1H; δ 8.39, d, 1H; δ 7.82, s, 1H; δ 7.48, d, 2H; δ 6.96, d, 2H; δ 4.36, m, 1H; δ 3.77, s, 3H; δ 3.29, m, 1H; δ 3.20, m, 2H; δ 3.07, m, 1H; δ 1.98, m, 1H; δ 1.84, m, 4H; δ 1.59, m, 1H), LC/MS (APCI, ES, M+H=389).

1. customDue to the hygroscopic nature of the salt form, the solvent was removed under vacuum
2. dissolutionThe residue was dissolved in methanol
3. concentrationconcentrated under vacuum (2×)
4. customto yield
5. customRecrystallization