反应详情

温度

0 °C

4-[2-(2,4-Dichloro-phenoxy)-phenylcarbamoyl]-piperidine-1-carboxylic acid tert-butyl ester (AMR01046, 1.0 g, 2.15 mmol) was dissolved in DCM (20 ml), and cooled to 0° C. and to this was added TFA (5 ml). This was allowed to warm to room temperature and stirred for 30 min. The reaction mixture was poured onto solid potassium carbonate (12 g), and water (50 ml) added. Extracted with DCM and the organic layers dried over anhydrous magnesium sulphate, and evaporated in-vacuo, to afford a cream oil, 0.77 g, 98%. R.f. 0.2 (EtOAc) 1HNMR (CDCl3, 300 MHz) δ 1.72 (2H, m, CH2), 1.87 (2H, m, CH2), 2.39 (1H, m, CH), 2.68 (2H, td, J=2.7, 12.3 Hz, CH2), 3.16 (2H, dt, J=3.6, 7.2, 12.6 Hz, CH2), 6.66 (1H, dd, J=1.5, 8.1 Hz, ArH), 6.87 (1H, d, J=8.7 Hz, ArH), 6.94 (1H, td, J=1.8, 8.1 Hz, ArH), 7.07 (1H, td, J=1.2, 7.8 Hz, ArH), 7.15 (1H, dd, J=2.7, 9.0 Hz, ArH), 7.43 (1H, d, J=2.4 Hz, ArH), 8.34 (1H, dd, J=6.9 Hz, ArH).

1. temperatureto warm to room temperature
2. additionadded
3. extractionExtracted with DCM
4. dry with materialthe organic layers dried over anhydrous magnesium sulphate
5. customevaporated in-vacuo
6. customto afford a cream oil, 0.77 g, 98%