反応 #1135821

反応方程式

2-Methylresorcinol

4-Hydroxyphenylacetic acid

BF3.OEt2

→

1-(2,4-Dihydroxy-3-methyl-phenyl)-2-(4-hydroxy-phenyl)-ethanone

反応条件

後処理

1. 1
   その他The round bottom flask was attached to a condenser
2. 2
   その他placed in an oil bath
3. 3
   その他A yellow solid formed at 20 minutes
4. 4
   workup.WAITThe reaction was left
5. 5
   温度on heat for a further 10 minutes
6. 6
   温度cooled to room temperature
7. 7
   ろ過The yellow solid was collected by suction filtration
8. 8
   洗浄washed with distilled water (200 ml)
9. 9
   その他to remove any excess BF3.OEt2 present
10. 10
    その他The solid was dried on a freeze dryer for 24 hours (8.93 g, 99%)

実験手順

2-Methylresorcinol (4.00 g, 1 equivalent) and 4-Hydroxyphenylacetic acid (5.00 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 BF3.OEt2 (20 ml, 5 equiv.) was added to the mixture while stirring. The mixture was refluxed (110° C.). A yellow solid formed at 20 minutes indicating that the reaction had gone to completion. The reaction was left on heat for a further 10 minutes and then 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-(4-hydroxy-phenyl)-ethanone in >95% purity. The solid was dried on a freeze dryer for 24 hours (8.93 g, 99%).

出典