反应详情

温度

110 °C

A mixture of 3.9 parts of 3-chloro-6-[4-(2-chloroethyl) 1-piperidinyl]pyridazine, 2.64 parts of (2-propynyl) 4-hydroxybenzoate, 2.76 parts of potassium carbonate and 75 parts of N,N-dimethylacetamide was stirred overnight at 110° C. After cooling the reaction mixture was poured into 100 parts of water and the product was extracted with methylbenzene. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98.2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 5.2 parts (86.7%) of (2-propynyl) 4-[2-[1-(6-chloro-3-pyridazinyl) -4-piperidinyl]ethoxy]benzoate; mp. 122.0° C. (comp. 120).

1. temperatureAfter cooling the reaction mixture
2. extractionthe product was extracted with methylbenzene
3. customThe extract was dried
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by column chromatography over silica gel using
7. additiona mixture of trichloromethane and methanol (98.2 by volume) as eluent
8. customThe pure fractions were collected
9. customthe eluent was evaporated
10. customThe residue was crystallized from 2-propanol
11. filtrationThe product was filtered off
12. customdried