反应详情

温度

65 °C

97.5 g (0.51 mole) of the sodium salt of 5-nitroguaiacol was dissolved in one liter of DMF and 1.5 equivalents of allyl bromide added. The reaction was heated to 65° C. for two hours, after which time much of the dark color had discharged and tlc (1:1 CH2Cl2/hexane) indicated loss of starting material. The solvent was concentrated in vacuum and the residue washed with water. The product was isolated by filtration and dried in a vacuum. This gave 112 g of pale yellow solid. A sample recrystallized from methanol, gave m.p. 93-94° C.

1. concentrationThe solvent was concentrated in vacuum
2. washthe residue washed with water
3. customThe product was isolated by filtration
4. customdried in a vacuum
5. customA sample recrystallized from methanol
6. customgave m.p. 93-94° C.