反应详情

A total of 662.4 g of potassium carbonate, 1161.2 g of 1,2-dichloroethane, 696.7 g of N,N-dimethylacetamide, 33.2 g of potassium iodide, and 464.5 g of methyl acetoacetate were mixed, followed by a reaction at 100° C. for 13 hours. The reaction mixture was cooled to room temperature and was filtrated, the resulting filtrate was washed with two portions of 5% by weight hydrochloric acid, and the organic layer was washed with water. The washing with the aqueous layer was extracted with 999.7 g of 1,2-dichloroethane. The extract with the organic layer was concentrated under a reduced pressure to distill off 1,2-dichloroethane, was subjected to distillation under a reduced pressure and thereby yielded 160.1 g of methyl 1-acetyl-1-cyclopropanecarboxylate as a colorless liquid as a fraction at 75° C./20 mmHg.

1. customfollowed by a reaction at 100° C. for 13 hours
2. filtrationwas filtrated
3. washthe resulting filtrate was washed with two portions of 5% by weight hydrochloric acid
4. washthe organic layer was washed with water
5. extractionThe washing with the aqueous layer was extracted with 999.7 g of 1,2-dichloroethane
6. extractionThe extract with the organic layer
7. concentrationwas concentrated under a reduced pressure
8. distillationto distill off 1,2-dichloroethane
9. distillationwas subjected to distillation under a reduced pressure