反応 #6608

反応方程式

sodium sulfate

4-cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether

lithium aluminum hydride

water

→

4-Aminomethylbenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetra-methyl-2-naphthyl ether

溶媒

ether

ether

反応条件

後処理

1. 1
   温度under reflux for 3 h
2. 2
   温度cooled
3. 3
   抽出The mixture was extracted three times with ether
4. 4
   洗浄the combined ether extracts were washed with water
5. 5
   乾燥dried over Na2SO4
6. 6
   濃縮concentrated

実験手順

A suspension of 3 g (9.4 mmol) of 4-cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether in 60 ml of ether was added dropwise under nitrogen to a suspension of 1 g (26 mmol) of lithium aluminum hydride in 50 ml of dry ether at 25° C. The mixture was then stirred under reflux for 3 h, cooled and hydrolyzed cautiously with water and sodium sulfate solution. The mixture was extracted three times with ether, and the combined ether extracts were washed with water, dried over Na2SO4 and concentrated. 3 g of the title compound of melting point 77°-79° C. remained.

出典