تفاعل #417899

معادلة التفاعل

ethylene glycol

3,5-Di-tert-butylhydroquinone

1,2-dibromoethane

potassium carbonate

→

title compound

5,7-di-tert-butyl-1,4-benzodioxin

المذيبات

Water

ظروف التفاعل

المعالجة

1. 1
   أخرىto quench
2. 2
   أخرىthe reaction
3. 3
   استخلاصthe organic compound was extracted by CH2Cl2
4. 4
   تركيزThe resulting solution was concentrated
5. 5
   أخرىto afford a crude oil
6. 6
   أخرىThe crude oil was then chromatographed (silica, hexane/ethyl acetate=20:1) mixture

الإجراء التجريبي

3,5-Di-tert-butylhydroquinone (3.33 g, 15 mmol) was combined with 1,2-dibromoethane (5.6 g), potassium carbonate (4.35 g) and ethylene glycol (25 mL). The mixture was heated in a 120° C. oil bath under an Ar atmosphere for 12 h. Water was added to the reaction mixture to quench the reaction and then the organic compound was extracted by CH2Cl2. The resulting solution was concentrated to afford a crude oil. The crude oil was then chromatographed (silica, hexane/ethyl acetate=20:1) mixture to afford the title compound (Rf=0.5, 5:1 hexane/ethyl acetate). 1H NMR (500 MHz, CDCl3): δ 7.03 (d, J=2 Hz, 1H), 6.93 (d, J=2 Hz, 1H), 4.34 (s, 4H), 1.53 (s, 9H), 1.43 (s, 9H).

المصدر