반응 #461523

반응 방정식

hexane ethyl acetate

2-acetylcyclohexanone

potassium carbonate

tert-butyl acrylate

→

2-Acetyl-2-[2-(tert-butoxycarbonyl)ethyl]cyclohexanone

용매

toluene

water

toluene

반응 조건

후처리

1. 1
   기타the layers separated
2. 2
   추출The aqueous layer was extracted with toluene (3×500 ml)
3. 3
   건조the combined toluene extracts dried over magnesium sulphate
4. 4
   여과filtered
5. 5
   농축concentrated under reduced pressure
6. 6
   기타to give a brown oil, (197.8 g) Rf
7. 7
   기타The crude product was used without further purification

실험 절차

To a suspension of 2-acetylcyclohexanone (100 g, 0.71 mol), potassium carbonate (118.3 g, 0.85 mol) and benzyltriethylammonium chloride (3.18 g, 0.014 mol) in toluene (280 ml), was added, in one portion, tert-butyl acrylate (137.1 g, 155.2 ml, 1.07 mol) at room temperature. The suspension was stirred at 40° C. for 18 hours, diluted with distilled water (1 L) and toluene (500 ml), and the layers separated. The aqueous layer was extracted with toluene (3×500 ml), the combined toluene extracts dried over magnesium sulphate, filtered and concentrated under reduced pressure to give a brown oil, (197.8 g) Rf. 0.41 (silica, hexane/ethyl acetate, 3:1). The crude product was used without further purification.

출처