반응 #1702069

반응 방정식

5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene

dichloromethane

aluminum chloride

isobutyryl chloride

→

5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl isopropyl ketone

용매

water

반응 조건

후처리

1. 1
   추출extracted by ethyl acetate
2. 2
   세척The organic layer was washed by water
3. 3
   건조a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
4. 4
   농축concentrated under reduced pressure
5. 5
   기타The crude product was purified by silica gel chromatography

실험 절차

The synthesis process is as set forth in the chemical reaction formula below. To 5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (188 mg, 1.00 mmol) were added anhydrous dichloromethane (1 mL), aluminum chloride (140 mg, 1.05 mmol), and isobutyryl chloride (112 mg, 1.05 mmol) followed by stirring at room temperature for 3 hours. The reaction solution was poured into cold water and extracted by ethyl acetate. The organic layer was washed by water, a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography using hexane/ethyl acetate (20/1) as an elution solvent. The yield was 97.4 mg (38%).

출처