تفاعل #94911

معادلة التفاعل

sesamol

α,α-dimethylbenzyl alcohol

oxalic acid

acetic acid

→

(α,α-Dimethylbenzyl)-3,4-methylenedioxy-6-methoxybenzene

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for 2.5 hours
2. 2
   استخلاصextracted with chloroform
3. 3
   workup.DISTILLATIONDistillation of the chloroform
4. 4
   استخلاصextract
5. 5
   أخرىgave an oil, b.p. 160°-163° at 0.5 mm Hg (60 g) which
6. 6
   أخرىcrystallized from aqueous methanol
7. 7
   أخرىto give colorless needles, m.p. 75°-76°

الإجراء التجريبي

(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 (3 g), 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.

المصدر