反应详情

50 cm3 of aqueous 4N sodium hydroxide solution are added slowly to a suspension of 20 g of (3aRS,7aRS)-7,7-diphenylperhydroisoindol-4-one hydrochloride in 250 cm3 of ethyl acetate, while stirring; stirring is continued until the starting material has disappeared. The organic solution is washed with 100 cm3 of distilled water and with 100 cm3 of a saturated solution of sodium chloride, dried over magnesium sulphate and filtered. A solution of 9.3 g of D-(-)-mandelic acid in 50 cm3 of ethyl acetate is added to the solution thus obtained, while stirring. The crystals formed are filtered filtered off, washed with 50 cm3 of ethyl acetate (twice) and dried. The crystals are taken up in a solution of 220 cm3 of acetonitrile and 60 cm3 of distilled water and the mixture is refluxed for 15 minutes, while stirring; the crystals formed are filtered off and crystallized again in a mixture of 100 cm3 of acetonitrile and 35 cm3 of distilled water. 6.4 g of (3aS,7aS)-7,7-diphenylperhydroisoindol-4-one D-mandelate are obtained.

1. stirringstirring
2. washThe organic solution is washed with 100 cm3 of distilled water and with 100 cm3 of a saturated solution of sodium chloride
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. additionA solution of 9.3 g of D-(-)-mandelic acid in 50 cm3 of ethyl acetate is added to the solution
6. customthus obtained
7. stirringwhile stirring
8. customThe crystals formed
9. filtrationare filtered
10. filtrationfiltered off
11. washwashed with 50 cm3 of ethyl acetate (twice) and
12. customdried
13. temperaturethe mixture is refluxed for 15 minutes
14. stirringwhile stirring
15. customthe crystals formed
16. filtrationare filtered off
17. customcrystallized again in a mixture of 100 cm3 of acetonitrile and 35 cm3 of distilled water