反应详情

cis-(Octahydro-quinolin-1-yl)-(5-piperidin-4-yl-thiophen-3-yl)-methanone (CC-033) (0.04 g, 0.12 mmol) was dissolved in dichloromethane (2 mL) and triethylamine (0.37 mmol). Methyl chloroformate (0.25 mmol) was added and the mixture stirred for 2 hours and then the solvent removed by evaporation. The residue was purified by HPLC, eluting with 10%-98% acetonitrile in water (0.1% formic acid). The fractions containing the desired product were concentrated under vacuum to give the title compound as a colourless oil (0.023 g). LCMS m/z 391.15 min [M+H]+ RT=11.55 min (Analytical Method 2). 1H NMR (400 MHz, CHCl3-d): δ 7.2 (s, 1H), 6.9 (s, 1H), 4.6 (m, 1H), 4.3 (m, 2H), 3.8 (m, 1H), 3.7 (s, 3H), 3.1-2.7 (m, 4H), 2.1-1.1 (m, 17H).

1. customthe solvent removed by evaporation
2. customThe residue was purified by HPLC
3. washeluting with 10%-98% acetonitrile in water (0.1% formic acid)
4. additionThe fractions containing the desired product
5. concentrationwere concentrated under vacuum