반응 #1135826

반응 방정식

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

반응 조건

후처리

1. 1
   기타The round bottom flask was attached to a condenser
2. 2
   기타placed in an oil bath
3. 3
   기타A yellow solid formed at 75 minutes
4. 4
   온도The reaction was heated for a further 10 minutes
5. 5
   온도cooled to room temperature
6. 6
   여과The yellow solid was collected by suction filtration
7. 7
   세척washed with distilled water (200 ml)
8. 8
   기타to remove any excess BF3.OEt2 present
9. 9
   기타The solid was dried on a freeze dryer for 24 hours (6.303 g, 43%)

실험 절차

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%).

출처