反应详情

To a solution of the product of step 2 (3.0 g) in THF (60 ml) was added 0.5 M KHMDS in toluene (108 ml) dropwise at −78° C. After the addition was completed, the mixture was kept at −78° C. for 40 minutes, then it was allowed to warm up slowly at room temperature. The mixture was quenched with H2O and the product was extracted twice with water. The combined aqueous layers were washed with ethyl acetate twice and then acidified with 6N HCl. The solid was filtered and the filter cake was washed with water and dried by vacuum aspiration to get a beige solid which was triturated into ethyl acetate to get a white solid (1.7 g). LRMS (ES+) m/z 230.05 (M+H)+.

1. additionAfter the addition
2. customThe mixture was quenched with H2O
3. extractionthe product was extracted twice with water
4. washThe combined aqueous layers were washed with ethyl acetate twice
5. filtrationThe solid was filtered
6. washthe filter cake was washed with water
7. customdried by vacuum aspiration
8. customto get a beige solid which
9. customwas triturated into ethyl acetate