反应详情

The crude [(2,6-dimethylphenyl)aminocarbonylmethyl]chloride, prepared in Preparation B (50 g., 0.25 moles) and 4-piperidone (86 g, 1 mole) are dissolved in 500 ml of ethanol. The mixture is refluxed for two hours, and then cooled and evaporated. The product is recovered by adding aqueous ammonia to the residue, and extracting with methylene chloride. Three portions of methylene chloride are used, which are collected, washed with water, and evaporated to a semi-solid. Upon addition of diethylether, the product crystallizes and is filtered. The resulting crude mixture is boiled with ether and then evaporated to a residue and triturated with hexane to yield pure material, 1-[(2,6-dimethylphenyl)aminocarbonylmethyl]-4-piperidone. This material is of sufficient purity for use in Reaction Sequences 2 to 5.

1. temperatureThe mixture is refluxed for two hours
2. temperaturecooled
3. customevaporated
4. customThe product is recovered
5. additionby adding aqueous ammonia to the residue
6. extractionextracting with methylene chloride
7. customwhich are collected
8. washwashed with water
9. customevaporated to a semi-solid
10. additionUpon addition of diethylether
11. customthe product crystallizes
12. filtrationis filtered
13. customevaporated to a residue
14. customtriturated with hexane