反応 #1702069

反応方程式

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

溶媒

water

反応条件

後処理

1. 1
   抽出extracted by ethyl acetate
2. 2
   洗浄The organic layer was washed by water
3. 3
   乾燥a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
4. 4
   濃縮concentrated under reduced pressure
5. 5
   その他The crude product was purified by silica gel chromatography

実験手順

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%).

出典