反応 #1702070

反応方程式

5,6,7,8-tetrahydro-3-hydroxy-5,5,8,8-tetramethyl-2-naphthyl methyl ketone

toluene

Lawesson's reagent

→

5,6,7,8-tetrahydro-3-hydroxy-5,5,8,8-tetramethyl-2-naphthyl ethanethione

溶媒

water

反応条件

後処理

1. 1
   抽出extracted by dichloromethane
2. 2
   濃縮the combined organic layers were concentrated under reduced pressure
3. 3
   その他The crude product was purified by silica gel column chromatography

実験手順

To 5,6,7,8-tetrahydro-3-hydroxy-5,5,8,8-tetramethyl-2-naphthyl methyl ketone (13.3 mg, 53.9 μmol) were added anhydrous toluene (1 mL) and Lawesson's reagent (32.0 mg, 80.9 mmol) followed by stirring at 120° C. for 24 hours. The reaction solution was poured into cold water and extracted by dichloromethane, and the combined organic layers were concentrated under reduced pressure. The crude product was purified by silica gel column chromatography using hexane/ethyl acetate (12/1) as an elution solvent. The yield was 4.2 mg (30%).

出典