反应详情

A solution of 13.2 g (50 mmol) of 3-(2-aminonaphthalen-1-yl)benzoic acid in 300 ml of THF is added dropwise to a solution of 3.8 g (100 mmol) of lithium aluminium hydride in 500 ml of THF. When the addition is complete, the mixture is stirred under reflux for a further 2 h and allowed to cool, 4 ml of water, 4 ml of 15% by weight NAOH solution and 12 ml of water are then added dropwise, the mixture is stirred for a further 30 min., the precipitated salts are filtered off with suction and washed three times with 100 ml of THF each time, and the THF is removed in vacuo. Yield: 11.2 g (90 mmol), 89.8%; purity according to 1H-NMR about 95%.

1. additionWhen the addition
2. temperatureunder reflux for a further 2 h
3. temperatureto cool
4. stirringthe mixture is stirred for a further 30 min.
5. filtrationthe precipitated salts are filtered off with suction
6. washwashed three times with 100 ml of THF each time
7. customthe THF is removed in vacuo