反应详情

温度

150 °C

A mixture of 19.3 parts of 3-chloro-6-methylpyridazine, 19.4 parts of 4-piperidinethanol, 16 parts of sodium carbonate and 0.85 parts of N,N-dimethylacetamide was stirred for 5 hours at 150° C. After cooling, the reaction mixture was diluted with water and extracted with dichloromethane (2×). The combined extracts were washed with water, dried, filtered and evaporated. The residue was purified by column chromatography (silica gel;CHCl3 /CH3OH 98:2). The eluent of the desired fraction was evaporated, yielding 23.6 parts (71.1%) of 1-(6-methyl-3-pyridazinyl)-4-piperidineethanol; p. 99°-100° C. at 8 Pa (interm. 24).

1. temperatureAfter cooling
2. extractionextracted with dichloromethane (2×)
3. washThe combined extracts were washed with water
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column chromatography (silica gel;CHCl3 /CH3OH 98:2)
8. customThe eluent of the desired fraction was evaporated