Реакция #1135826

Уравнение реакции

2-Methylresorcinol

3,4-dimethoxyphenylacetic acid

boron trifluoride diethyl etherate

BF3.OEt2

→

1-(2,4-dihydroxy-3-methyl-phenyl)-2-(3,4-dimethoxy-phenyl) ethanone

Условия реакции

Обработка

1. 1
   ДругоеThe round bottom flask was attached to a condenser
2. 2
   Другоеplaced in an oil bath
3. 3
   ДругоеA yellow solid formed at 75 minutes
4. 4
   ТемператураThe reaction was heated for a further 10 minutes
5. 5
   Температураcooled to room temperature
6. 6
   ФильтрацияThe yellow solid was collected by suction filtration
7. 7
   Промывкаwashed with distilled water (200 ml)
8. 8
   Другоеto remove any excess BF3.OEt2 present
9. 9
   ДругоеThe solid was dried on a freeze dryer for 24 hours (6.303 g, 43%)

Методика

2-Methylresorcinol (6.285 g, 1 equivalent) and 3,4-dimethoxyphenylacetic acid (9.251 g, 1 equivalent) were added to a round bottom flask. The round bottom flask was attached to a condenser and placed in an oil bath, the whole system was kept under nitrogen. Distilled boron trifluoride diethyl etherate, BF3.OEt2 (42 ml, 5 equiv.) was added to the mixture while stirring. The mixture was refluxed (110° C.). A yellow solid formed at 75 minutes indicating that the reaction had gone to completion. The reaction was heated for a further 10 minutes and cooled to room temperature. The yellow solid was collected by suction filtration and washed with distilled water (200 ml) to remove any excess BF3.OEt2 present. 1H NMR in d-DMSO indicated the yellow solid was 1-(2,4-dihydroxy-3-methyl-phenyl)-2-(3,4-dimethoxy-phenyl) ethanone in >95% purity. The solid was dried on a freeze dryer for 24 hours (6.303 g, 43%).

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