反应详情

To a mixture of dehydro-aripiprazole (1.5 g, 3.4 mmol), potassium tert-butoxide (0.75 g, 6.7 mmol) and 2-methyltetrahydrofuran (30 mL) at 0° C. was added hexyl chloroformate (1.32 mL, 8.1 mmol). The reaction mixture was stirred for 2 h, allowed to self warm to room temperature and stirred for a further 4 h. The reaction mixture was then diluted with water and extracted with ethyl acetate. The organic phase was dried over MgSO4, filtered and evaporated. The residue was further purified on silica eluting with ethyl acetate/tetrahydrofuran and the major product containing fractions evaporated to give a yellow solid. This was triturated in heptane (30 mL) for 2.5 h, filtered and dried to give Compound-328 (1.55 g) as a white solid.

1. stirringstirred for a further 4 h
2. extractionextracted with ethyl acetate
3. dry with materialThe organic phase was dried over MgSO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was further purified on silica eluting with ethyl acetate/tetrahydrofuran
7. additionthe major product containing fractions
8. customevaporated
9. customto give a yellow solid
10. customThis was triturated in heptane (30 mL) for 2.5 h
11. filtrationfiltered
12. customdried
13. customto give Compound-328 (1.55 g) as a white solid