反应详情

Add 68 ml of 3.6N aqueous sulfuric acid to a stirred solution of 40.0 g of 1-benzhydryl-2-benzimidoylazetidine in 800 ml. of methanol. Stir under a nitrogen atmosphere for 1.5 hours at room temperature. Slowly pour the mixture, with continuous stirring, into 234 ml. of 1.1N aqueous sodium bicarbonate. Filter the resultant solid, and extract the filter cake with methylene chloride. Combine the methylene chloride extracts with the methanolic filtrate and remove all solvent in vacuo. Dissolve the residual solid in ether, wash with water, and dry over anhydrous sodium sulfate. Remove the drying agent, concentrate the solution in vacuo to a volume of 350 ml. and triturate the solid which precipitates. Filter to obtain the analytically pure product, m.p. 114°-115° C.

1. additionSlowly pour the mixture
2. filtrationFilter the resultant solid
3. extractionextract the filter cake with methylene chloride
4. customremove all solvent in vacuo
5. dissolutionDissolve the residual solid in ether
6. washwash with water
7. dry with materialdry over anhydrous sodium sulfate
8. customRemove the drying agent
9. concentrationconcentrate the solution in vacuo to a volume of 350 ml
10. customand triturate the solid which
11. customprecipitates
12. filtrationFilter
13. customto obtain the analytically pure product, m.p. 114°-115° C.