反应详情

106 g of 2-methyl-5-(4-chlorobenzylidene)-cyclopentanone, 49.5 g of 85% strength aqueous potassium hydroxide solution, 8.3 g of potassium iodide and 400 g of tert-butanol were weighed in succession into a 700 ml stainless steel autoclave, and 50.5 g of methyl chloride were injected at 20° C. The mixture was stirred at room temperature for 23 hours and then 300 ml of tert-butanol were distilled off at 20 mbar up to an overhead temperature of max. 50° C. 400 ml of water were added to the residue, and the mixture was stirred thoroughly. The resulting suspension was filtered off over a suction filter, and the filter cake was washed twice with 200 ml of water each time and dried. 112.8 g of a pale beige solid were thus obtained with a purity of 89.5%. The yield of the crude product was 90.2% of theory.

1. customwere injected at 20° C
2. distillation300 ml of tert-butanol were distilled off at 20 mbar up to an overhead temperature of max
3. custom50° C
4. addition400 ml of water were added to the residue
5. stirringthe mixture was stirred thoroughly
6. filtrationThe resulting suspension was filtered off over a suction
7. filtrationfilter
8. washthe filter cake was washed twice with 200 ml of water each time
9. customdried