反应详情

温度

90 °C

In a reactor equipped with a stirrer and a thermometer, 5-decyloxy-2-(4-bromophenyl)pyrimidine (25 g), optically active 6-hydroxy-1-heptyne (8.58 g), dichlorobis(triphenylphosphine)palladium (0.1 g), copper iodide (0.1 g), triphenylphosphine (0.52 g) and triethylamine (200 ml) are charged and heated up to 90° C. to carry out a reaction for 10 hours. After evaporating triethylamine off under reduced pressure, toluene and 10% hydrochloric acid are added to the residue for extraction, and the organic layer is washed with water and evaporated under reduced pressure. A resulting residue is purified by silica gel column chromatography (eluent: hexane-ethyl acetate) to obtain (-)-5-decyloxy-2-[4-(6-hydroxyheptynyl)phenyl]-pyrimidine (23.4 g). [α]D20 =-3.3° (c=1.035, CHCl3).

1. customIn a reactor equipped with a stirrer
2. customa reaction for 10 hours
3. customAfter evaporating triethylamine off under reduced pressure, toluene and 10% hydrochloric acid
4. additionare added to the residue for extraction
5. washthe organic layer is washed with water
6. customevaporated under reduced pressure
7. customA resulting residue is purified by silica gel column chromatography (eluent: hexane-ethyl acetate)