反应详情

Dimethylformamide (600 ml), p-pentyloxyacetophenone (60.0 g) and dimethyl terephthalate (73.5 g) were charged in 1-liter three-necked flask and stirred. To this mixture was added 28% methanolic solution (84.2 g) of sodium methoxide and, after that, a reaction was carried out at the inner temperature of 35 to 40° C. for 48 hours. After completion of the reaction, the reaction solution was added to a mixed solution of water (3,000 ml) and 1N hydrochloric acid (600 ml) to separate the crystals. The mixture was stirred at room temperature for 1 hour, and then the separated crystals were filtered. The wet crystals and methanol (1,000 ml) were charged in a 2-liter three-necked flask, heated to reflux for 2 hours and cooled down to room temperature, and the crystals were filtered. The crystals were washed with methanol (200 ml). The crystals were dried overnight in vacuo to give 1-(4-methoxycarbonylphenyl)-3-(4-pentyloxyphenyl)-propane-1,3-dione (66.0 g).

1. customAfter completion of the reaction
2. customto separate the crystals
3. stirringThe mixture was stirred at room temperature for 1 hour
4. filtrationthe separated crystals were filtered
5. additionThe wet crystals and methanol (1,000 ml) were charged in a 2-liter three-necked flask
6. temperatureheated
7. temperatureto reflux for 2 hours
8. filtrationthe crystals were filtered
9. washThe crystals were washed with methanol (200 ml)
10. customThe crystals were dried overnight in vacuo