Реакция #432313

Уравнение реакции

2,3-dihydro-2,4,6-trimethyl-7-methoxy-2-benzyl-1H-inden-1-one

sodium iodide

aluminium chloride

→

2,3-dihydro-2,4,6-trimethyl-7-hydroxy-2-benzyl-1H-indene-1-one

Растворители

acetonitrile

Условия реакции

Обработка

1. 1
   ДругоеThen the solvent was removed by evaporation under a reduced pressure
2. 2
   Другоеthe residue thus obtained
3. 3
   Экстракцияwas extracted with ethyl acetate
4. 4
   ПромывкаThe extract was washed with an aqueous solution saturated with sodium chloride
5. 5
   Другоеan aqueous solution of sodium thiosulfate and an aqueous solution saturated with sodium chloride in this order, and the insoluble matters were removed by filtration
6. 6
   ДругоеThe solvent was removed by evaporation
7. 7
   Другоеthe residue thus obtained
8. 8
   Другоеwas recrystallized from n-hexane

Методика

23.0 Grams of 2,3-dihydro-2,4,6-trimethyl-7-methoxy-2-benzyl-1H-inden-1-one and 25.8 g of sodium iodide were dissolved in 90 ml of acetonitrile. To this solution was added 22.9 g of aluminium chloride at room temperature and stirred for 1 hour. Then the solvent was removed by evaporation under a reduced pressure, and the residue thus obtained was extracted with ethyl acetate. The extract was washed with an aqueous solution saturated with sodium chloride, an aqueous solution of sodium thiosulfate and an aqueous solution saturated with sodium chloride in this order, and the insoluble matters were removed by filtration. The solvent was removed by evaporation and the residue thus obtained was recrystallized from n-hexane to obtain 19.7 g of 2,3-dihydro-2,4,6-trimethyl-7-hydroxy-2-benzyl-1H-indene-1-one. Colorless prism-like crystals. Melting point: 86°-87° C.

Источник