تفاعل #1702070

معادلة التفاعل

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

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted by dichloromethane
2. 2
   تركيزthe combined organic layers were concentrated under reduced pressure
3. 3
   أخرىThe crude product was purified by silica gel column chromatography

الإجراء التجريبي

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%).

المصدر