反应详情

In a Soxhlet apparatus 18.4 g of lithium aluminium hydride in 1800 ml of dry ether are boiled under a nitrogen atmosphere at a bath temperature of 70°, 5.3 g of 2-benzyloxybenzamide being introduced into the Soxhlet thimble. After 21 hours the reaction mixture is immersed in an ice bath, and 18.4 ml of water, 18.4 ml of 15% sodium hydroxide solution and 55 ml of water are added dropwise in succession, whilst stirring. The temperature may be allowed to rise to a maximum of +10°. Stirring of the mixture is then continued at 20° and the resulting precipitate is suction-filtered and washed with ether. The filtrate is concentrated by evaporation in vacuo and the oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours, whilst cooling with ice. The precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered, washed with water and ether and dried in vacuo. Melting point 190°-191°.

1. customto rise to a maximum of +10°
2. stirringStirring of the mixture
3. customis then continued at 20°
4. filtrationthe resulting precipitate is suction-filtered
5. washwashed with ether
6. concentrationThe filtrate is concentrated by evaporation in vacuo
7. stirringthe oil remaining is stirred with 500 ml of 10% hydrochloric acid and 400 ml of ether for 2 hours
8. temperaturewhilst cooling with ice
9. filtrationThe precipitated 2-benzyloxybenzylamine hydrochloride is suction-filtered
10. washwashed with water and ether
11. customdried in vacuo