background and overview[1]
4-morpholinopropiophenone can be used as a pharmaceutical synthesis intermediate. if 4-morpholinopropiophenone is inhaled, move the patient to fresh air; if skin contact occurs, take off contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical attention if you feel unwell; if contact with eyes , you should separate your eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse your mouth immediately, do not induce vomiting, and seek medical attention immediately.
preparation[1]
4-morpholinopropiophenone is prepared as follows:
the specific steps are as follows: add a mixture of 1-(4-fluorophenyl)ethanone (5g, 36.20mmol), morpholine (6.31g, 72.39mmol) and k2co3 (10g, 72.39mmol) in dmf at 100 stir overnight at ℃. the reaction mixture was cooled to ambient temperature and evaporated to remove the solvent. the residue was purified by silica gel column chromatography (4 × 16 cm, eluting with 10% ethyl acetate/petroleum ether) to give the title compound 4-morpholinopropiophenone (2.63 g, 35.4%) as a yellow solid. 1hnmr (300mhz, cdcl3) 68.40 (d, j=8.4hz, 2h), 8.70 (d, j=8.4hz, 2h), 3.88-3.85 (m, 4h), 3.33-3.29 (m, 4h), 2.53 ( s, 3h); lc-ms>95% (purity), 206 (mh)+.
application
4-morpholinopropiophenone can be used as a pharmaceutical synthesis intermediate. if the following reaction occurs:
the specific steps are as follows: cool the solution of 4-morpholinopropiophenone (5g, 24.36mmol) in concentrated sulfuric acid (30ml) to 0°c. bromine (1.28 ml, 25.09 mmol) was slowly added to the solution. the resulting mixture was gradually warmed to ambient temperature and stirred for a further 6 hours. pour the reaction mixture into ice water. the precipitate formed was filtered, washed with water and air dried to give the product as a green solid. lc-ms 363.9 (mh)+ (78%) and 442.8 (mh)+ (22%).
main reference materials
[1](wo2010028193)compoundsincludingpimelicacidderivativesashdacinhibitors
微信扫一扫打赏
