反応 #432109

反応方程式

sodium boron hydride

5'-acetyl-3,3'-diallyl-5-ethyl-2,4'-biphenyldiol

methylamine

sodium hydrogencarbonate

hydrochloric acid

sodium boron hydride

→

3,3'-diallyl-5-ethyl-5'-(1-methylaminoethyl)-2,4'-biphenyldiol

溶媒

metanol

water

反応条件

後処理

1. 1
   その他A solution was prepared
2. 2
   温度by heating for 3 hours
3. 3
   温度cooled
4. 4
   温度by heating
5. 5
   抽出extracted with diethylether
6. 6
   洗浄The extract was washed with an aqueous solution saturated with NaCl
7. 7
   乾燥dried with sodium sulfate
8. 8
   濃縮concentrated
9. 9
   その他The concentrate was purified by silica gel column-chromatography (dichloroethane:methanol=50:1)

実験手順

A solution was prepared by dissolving 0.10 g of 5'-acetyl-3,3'-diallyl-5-ethyl-2,4'-biphenyldiol into 2 ml of 40% metanol solution of methylamine. The solution was reflexed by heating for 3 hours, cooled, 0.2 g of sodium boron hydride was added thereinto, was reflexed by heating. The solution was added 0.2 g of sodium boron hydride and stirred from 1 hour at room temperature. The reaction mixture, wherein an excess of reagent was decomposed with hydrochloric acid, was neutralized with water solution of sodium hydrogencarbonate and extracted with diethylether. The extract was washed with an aqueous solution saturated with NaCl, dried with sodium sulfate and concentrated. The concentrate was purified by silica gel column-chromatography (dichloroethane:methanol=50:1) to yield 80 mg of 3,3'-diallyl-5-ethyl-5'-(1-methylaminoethyl)-2,4'-biphenyldiol.

出典