反应详情

With respect to 1 kg of the reaction solution generated in synthesis example 1, 1 L of toluene and 2 L of water were added. These components were stirred for 5 minutes and extraction was conducted. Then, the resultant substance was kept still for 15 to 20 minutes to be separated, and the upper toluene layer was recovered. The above-extracted solution and the same amount of 4% aqueous solution of sodium hydroxide were put into a separatory funnel, shaken and kept still. Then, the lower black liquid was removed. The remaining liquid was washed with water of the same amount as that of the remaining liquid. Then, the lower layer was removed. Water was added, 2 mL of hydrochloric acid was added, and these components were shaken. The lower layer was removed, and the remaining substance was washed with water again. The oil layer was washed with an alkaline substance and concentrated to remove the solvent. The concentrate was distilled at a pressure of 1 to 2 mmHg. As a result, 16 g of acenaphthene-1-one was obtained at a distillation temperature of 120° C.

1. additionwere added
2. extractionextraction
3. waitThen, the resultant substance was kept still for 15 to 20 minutes
4. customto be separated
5. customthe upper toluene layer was recovered
6. customThe above-extracted solution and the same amount of 4% aqueous solution of sodium hydroxide were put into a separatory funnel
7. stirringshaken
8. customThen, the lower black liquid was removed
9. washThe remaining liquid was washed with water of the same amount as that of the remaining liquid
10. customThen, the lower layer was removed
11. additionWater was added
12. addition2 mL of hydrochloric acid was added
13. stirringthese components were shaken
14. customThe lower layer was removed
15. washthe remaining substance was washed with water again
16. washThe oil layer was washed with an alkaline substance
17. concentrationconcentrated
18. customto remove the solvent
19. distillationThe concentrate was distilled at a pressure of 1 to 2 mmHg