反应详情

According to the described procedure of Carr et al., U.S. Pat. No. 4,254,129, to a solution of 0.6 g of ethyl 4-[4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-hydroxybutyl]-α,α-dimethylbenzeneacetate in 20 ml of absolute ethanol is added 10 ml of a 50% solution of sodium hydroxide. The mixture is refluxed for 3½ hours and concentrated to a solid after which a minimum amount of methanol to dissolve the residue is added. 10% Aqueous HCl is added until pH 7 is reached, the methanol removed by evaporation and water (25 ml) is added. The resulting precipitate is recrystallized from methanolbutanone to give 4-[4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-hydroxybutyl]-α,α-dimethylbenzeneacetic acid, M.P. 195°-197° C.

1. temperatureThe mixture is refluxed for 3½ hours
2. concentrationconcentrated to a solid after which a minimum amount of methanol
3. dissolutionto dissolve the residue
4. additionis added
5. addition10% Aqueous HCl is added until pH 7
6. customthe methanol removed by evaporation and water (25 ml)
7. additionis added
8. customThe resulting precipitate is recrystallized from methanolbutanone