反应详情

(α,α-Dimethylbenzyl)-3,4-methylenedioxy-6-methoxybenzene was prepared as follows: A mixture of sesamol (44 g), α,α-dimethylbenzyl alcohol (44 g), oxalic acid (3g), acetic acid (100 ml) and water (10 ml) was refluxed for 2.5 hours, diluted with water and extracted with chloroform. Distillation of the chloroform extract gave an oil, b.p. 160°-163° at 0.5 mm Hg (60 g) which crystallized from aqueous methanol to give colorless needles, m.p. 75°-76° (Found: C, 75.0; H, 6.26. Calc. for C16H16O3 : C, 75.0; H, 6.29%); pmr spectrum: δ1.63, 6H, S; 4.12, 1H, S; δ5.81, 2H, S; δ6.33, 1H, S; δ6.98, 1H, S; δ6.31, 5H, S.

1. temperaturewas refluxed for 2.5 hours
2. extractionextracted with chloroform
3. distillationDistillation of the chloroform
4. extractionextract
5. customgave an oil, b.p. 160°-163° at 0.5 mm Hg (60 g) which
6. customcrystallized from aqueous methanol
7. customto give colorless needles, m.p. 75°-76° (Found: C, 75.0; H, 6.26. Calc. for C16H16O3 : C, 75.0; H, 6.29%)