反应详情

Methyl ester 18 (3.20 g, 9.16 mmol) was dissolved in THF (30 mL) and NaOH (0.552 g, 13.8 mmol) dissolved in water (10 mL) was added. Methanol (10 mL) was added to obtain a homogenous solution and this was stirred at rt for 18 h. The reaction mixture was then concentrated in vacuo and the residue was partitioned between EtOAc and 1M hydrochloric acid. The aqueous phase was extracted twice more with EtOAc and the combined organic extracts were washed with brine, dried (MgSO4), filtered and concentrated in vacuo to yield a white solid, 2.60 g, 85%. m.p. 148-150° C.

1. additionwas added
2. customto obtain a homogenous solution
3. concentrationThe reaction mixture was then concentrated in vacuo
4. customthe residue was partitioned between EtOAc and 1M hydrochloric acid
5. extractionThe aqueous phase was extracted twice more with EtOAc
6. washthe combined organic extracts were washed with brine
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customto yield a white solid, 2.60 g, 85%