Реакция #1702070
ord-93356178ab5f4aeeb11449bfb9ef3de0
Уравнение реакции
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
Реактанты
Реагенты
Нет
Растворители
Условия реакции
Температура
120°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Экстракцияextracted by dichloromethane
- 2Концентрированиеthe combined organic layers were concentrated under reduced pressure
- 3ДругоеThe crude product was purified by silica gel column chromatography
Методика
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%).