反应详情

To a solution of indene-3-ethanol (8 g) and methyl acetoacetate (6 g) in 250 ml of dry benzene containing hydrated alkali-aluminum silicate (Molecular Sieves No. 4, about 2 g) is added 1 ml of boron trifluoride-etherate and the mixture stirred at room temperature for 4 hr. An additional 1 ml of boron trifluoride-etherate is added, the reaction mixture is stirred at ambient temperature overnight and then heated at reflux for 1 hr. The hydrated alkali-aluminum silicate is collected and the filtrate washed with 10% solution of sodium bicarbonate and water. After drying over magnesium sulfate the benzene is removed under reduced pressure affording 1-methyl-1,3,4,9-tetrahydroindeno[2,1-c]pyran-1-acetic acid methyl ester, νmaxfilm 1724 cm-1.

1. stirringthe reaction mixture is stirred at ambient temperature overnight
2. temperatureheated
3. temperatureat reflux for 1 hr
4. customThe hydrated alkali-aluminum silicate is collected
5. washthe filtrate washed with 10% solution of sodium bicarbonate and water
6. dry with materialAfter drying over magnesium sulfate the benzene
7. customis removed under reduced pressure