2-Propanone, 1-(acetyloxy)-3-chloro- → HCID 25261017, compound

Participants

Reaction Conditions

Reaction Steps

(5-Phenoxy-pyridine-2-yl)-thiourea (0.86 mmol) is dissolved in DMF (1 ml) and acetic acid 3-chloro-2-oxo-propyl ester (1.1 eq.) in 1 ml DMF is added and stirred 2 h at 70° C. After cooling to RT the precipitate is filtered, washed with water and dried 16 h in vacuo at 40° C. “A9” is obtained after column chromatography (heptan/ethyl acetate) as colourless powder in a yield of 69%; mp. 158.5-160.5° C.; HPLC (method C): 1.89 min; LC-MS (method A): 1.938 min, 342.15 (M+H+); 1H-NMR (DMSO-d6, 500 MHz): δ [ppm] 11.375 (s, 1H), 8.105 (d, 1H, J=2.8 Hz), 7.519 (dd, 1H, J=8.9 Hz, J=2.8 Hz), 7.389-7.347 (m, 2H), 7.120-7.088 (m, 2H), 6.995-6.978 (m, 2H), 6.918 (s, 1H), 5.007 (s, 2H), 2.064 (s, 3H).

Provenance & Evidence