反应详情

温度

25 °C

Specifically, first, a mixture liquid was obtained by feeding 73 g (0.5 mol) of α-tetralone, 47.3 g (0.55 mol) of a 37% by mass aqueous formalin solution, and 45 g (0.55 mol) of dimethylamine hydrochloride to a 500-ml three-necked flask. Next, a bulb condenser was set to the three-necked flask, and then the inside atmosphere of the three-necked flask was replaced with nitrogen. Thereafter, the three-necked flask was immersed in an oil bath of 100° C., and the mixture liquid was stirred for 60 minutes with heating. After thus stirred, the mixture liquid was cooled with ice to 25° C., and was washed twice with diethyl ether (twice with 30 ml each). Subsequently, the thus washed mixture liquid was allowed to stand one day and one night (24 hours). White crystals formed in the mixture liquid were separated by filtration, and washed with acetone. The thus obtained white crystals were vacuum dried. Thus, 12.9 g of N,N-dimethylaminomethyl-1-tetralone hydrochloride was obtained (yield: 11%). Note that the thus obtained compound was subjected to NMR measurement. As a result, it was found that a purity of N,N-dimethylaminomethyl-1-tetralone hydrochloride was 85.7%, and that 14.3% of dimethylamine hydrochloride was included as a by-product.

1. customSpecifically, first, a mixture liquid was obtained
2. customNext, a bulb condenser was set to the three-necked flask
3. customThereafter, the three-necked flask was immersed in an oil bath of 100° C.
4. temperaturewith heating
5. stirringAfter thus stirred
6. washwas washed twice with diethyl ether (twice with 30 ml each)
7. waitto stand one day and one night
8. custom(24 hours)
9. customWhite crystals formed in the mixture liquid
10. customwere separated by filtration
11. washwashed with acetone
12. customdried