反应详情

温度

68 °C

Dissolve 4-[4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate (69.0 g, 0.131 mol) in methanol (2.5 L) and add 10% aqueous sodium hydroxide (769 mL, 1.92 mol). Stir at reflux for 1.5 hours, cool to 68° C. and evaporate the solvent in vacuo to a residue (700 mL). Add chloroform (1 L) and stir until solids are dissolved. Separate the organic phase and extract the aqueous phase with chloroform (3×300 mL). Combine the organic phases, dry (MgSO4) and evaporate the solvent in vacuo and recrystallize (toluene) to give the title compound as a cream-colored powder; mp 135°-137° C.

1. temperatureat reflux for 1.5 hours
2. customevaporate the solvent in vacuo to a residue (700 mL)
3. stirringAdd chloroform (1 L) and stir until solids
4. dissolutionare dissolved
5. customSeparate the organic phase
6. extractionextract the aqueous phase with chloroform (3×300 mL)
7. dry with materialCombine the organic phases, dry (MgSO4)
8. customevaporate the solvent in vacuo
9. customrecrystallize (toluene)