反应详情

温度

140 °C

6-Chloro-5-cyclopropyl-2-pyridinecarboxylic acid (CAN 1211530-95-8; 180 mg, 901 μmol), (S)-4,4,4-trifluorobutane-1,3-diol (394 mg, 2.73 mmol) and potassium tert-butoxide (307 mg, 2.73 mmol) were combined with DMF (3 mL) to give a white suspension. The reaction mixture was heated to 140° C. and stirred for 48 h. After cooling the mixture was poured into cold 1 M HCl (15 mL) and extracted with ethyl acetate (2×75 mL). The phases were combined, dried with Na2SO4 and concentrated in vacuo. The residue was purified by preparative HPLC to give the title compound (23 mg, 8.3%) and its regioisomer; MS (EI) 304.2 (M+H)+.

1. customto give a white suspension
2. temperatureAfter cooling the mixture
3. extractionextracted with ethyl acetate (2×75 mL)
4. dry with materialdried with Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by preparative HPLC