反应详情

The intermediate t-butyl octahydro-3-oxo-1H-isoindole-1-carboxylate is prepared from octahydro-3-oxo-1H-isoindole-carboxylic acid (Example 5) as follows. A mixture of 10 g of this acid and 0.4 ml of 70% perchloric acid in 150 ml of t-butyl acetate is allowed to stand for 2.5 days. An additional 50 ml of t-butyl acetate is added and the reaction is allowed to continue for 15 days. The solution is filtered and poured onto 14 g of 50% sodium hydroxide solution and ice. The product is extracted into ether. Drying and concentration gives a residue which when triturated with hexane gives material, mp 143°-149° C., suitable for further use.

1. waitto continue for 15 days
2. filtrationThe solution is filtered
3. additionpoured onto 14 g of 50% sodium hydroxide solution and ice
4. extractionThe product is extracted into ether
5. customDrying
6. concentrationconcentration
7. customgives a residue which when
8. customtriturated with hexane
9. customgives material, mp 143°-149° C.