The brand new solvent is actually removed under shorter tension, drinking water was added additionally the resulting mix try removed that have EtOAc
General procedure for the preparation of benzamides 2, cuatro, and 21–2step step step step three: To a mixture of the appropriate acid (1 equiv) and 20 (1 equiv) in CH2Cl2 (5 mL mmol ?1 ) was added HATU (1.2 equiv) and DIPEA (3 equiv) at 0 °C and after which it was stirred at 30 °C for 8 h. The combined organic layers were dried over anhydrous Na2SO4 and filtered. The EtOAc was evaporated under reduced pressure and the resulting crude product was purified by column chromatography over SiO2 (hexane/EtOAc as eluent) to afford the desired amides 2, 4, 21–23.
This new solvent are evaporated under smaller stress and the ensuing rough device refined of the column chromatography toward SiO
Ethyl 3-(3,4-dimethoxy-benzamido)benzoate (2): Compound 2 was synthesized according to the general kenyancupid iÅŸe yarıyor mu procedure by using 19 (0.05 g, 0.twenty eight mmol) and was obtained as a yellow solid (0.63 g, 0.21 mmol, 76 %). 1 H NMR (400 MHz, CDCl3): ?=8.19–8.00 (m, 3H), 7.80 (d, J=7.5 Hz, 1H), 7.49 (s, 1H), 7.47–7.37 (m, 2H), 6.87 (d, J=8.4 Hz, 1H), 4.35 (q, J=7.1 Hz, 2H), 3.92 (s, 6H), 1.37 (t, J=7.0 Hz, 3H). 13 C NMR (101 MHz, CDCl3): ?=, , , , , , , , , , , , , , , , ; HRMS (ESI + ) [M+H] + C18NO5 calculated Da, found: m/z. (more…)