反应详情

In a two liter three neck round bottom flask (argon atmosphere) was placed 300 ml of dry THF and 30.06 g (0.8 mole) of LAH was added cautiously. The reaction mixture was stirred and a suspension of 89.31 g (0.4 mole) of 11,12-dihydrodibenz[b,f]azocin-6(5H)-one (Aldrich) in 400 ml of hot THF was added dropwise. After the addition, the reaction mixture was stirred and heated to reflux for 8.5 hr. The reaction mixture was cooled to RT and 60 ml of 1N sodium hydroxide was added with caution (hydrogen evolution). The reaction mixture was stirred and heated to reflux for 0.5 hr to give a white suspension. The solid was removed by filtration and washed with several portions of warm THF. The filtrate was concentrated to dryness in vacuo to give 82.5 g of white solid title compound of 99.5% purity by g.c. The product was used in the next step without further purification.

1. additionwas added cautiously
2. additionwas added dropwise
3. additionAfter the addition
4. stirringthe reaction mixture was stirred
5. temperatureheated
6. temperatureto reflux for 8.5 hr
7. stirringThe reaction mixture was stirred
8. temperatureheated
9. temperatureto reflux for 0.5 hr
10. customto give a white suspension
11. customThe solid was removed by filtration
12. washwashed with several portions of warm THF
13. concentrationThe filtrate was concentrated to dryness in vacuo