Реакция #42759

Уравнение реакции

2′,4′-Dihydroxyacetophenone

4-methoxybenzyl chloride

potassium carbonate

potassium iodide

→

1-[2-Hydroxy-4-(4-methoxy-benzyloxy)-phenyl]ethanone

Растворители

acetone

water

Условия реакции

Обработка

1. 1
   Экстракцияextracted with ethyl acetate (3×100 ml)
2. 2
   Промывкаwashed with saturated brine (100 ml)
3. 3
   Сушкаdried (MgSO4)
4. 4
   Фильтрацияfiltered
5. 5
   Концентрированиеconcentrated, until crystallization commences
6. 6
   Фильтрацияthe crystals are recovered by filtration
7. 7
   Промывкаwashed with cold ethyl acetate
8. 8
   Сушкаwith n-hexane and dried

Методика

2′,4′-Dihydroxyacetophenone (11.71 g, 0.077 mol), 4-methoxybenzyl chloride (10.44 ml, 0.077 mol), anhydrous potassium carbonate (11.75 g, 0.085 mol) and potassium iodide (12.78 g, 0.077 mol) are heated together in refluxing dry acetone (80 ml) for 4 hours. The mixture is then cooled to room temperature, poured into water (250 ml) and extracted with ethyl acetate (3×100 ml). The ethyl acetate extracts are combined, washed with saturated brine (100 ml), dried (MgSO4), filtered and concentrated, until crystallization commences. After standing at 4° C. for 16 h, the crystals are recovered by filtration, washed with cold ethyl acetate and then with n-hexane and dried.

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