反应详情

温度

100 °C

A mixture of 548 g of lithium carbonate and 548 of lithium bromide in 5.480 liters of dimethylformamide was heated to 100° C. and 548 g of 3-nitro-6-bromo-6,7,8,9-tetrahydro [5H] benzocycloheptene-5-one were added thereto over 5 minutes. The mixture was held at 100° C. for 45 minutes and was then poured into 25 liters of a mixture of water and ice. The mixture was vacuum filterd and the insolubles were extracted 8 times with 1 liter of methylene chloride. The organic phase was washed with water, dried over sodium sulfate and was evaporated to dryness under reduced pressure to obtain a red crystalline mass. The latter was empasted successively 3 times with 400 ml of ether, once with 400 ml of ethanol and once with 400 ml of ether and was dried at 40° C. to obtain 286.7 g of 3-nitro-8,9-dihydro [5H] benzocycloheptene-5-one in the form of orange-red crystals melting at 128° C.

1. waitThe mixture was held at 100° C. for 45 minutes
2. extractionthe insolubles were extracted 8 times with 1 liter of methylene chloride
3. washThe organic phase was washed with water
4. dry with materialdried over sodium sulfate
5. customwas evaporated to dryness under reduced pressure
6. customto obtain a red crystalline mass
7. dry with materialonce with 400 ml of ethanol and once with 400 ml of ether and was dried at 40° C.