反应详情

To a solution of 3-methylsulfanyl-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid methyl ester (B1) (115 mg, 0.433 mmol, 1 equiv) in MeOH (8 ml) was added 2N aqueous NaOH solution (0.65 ml, 1.3 mmol, 3 equiv). The resulting mixture was stirred for 4 h, 2N aqueous NaOH solution (1 ml, mmol, equiv) was added and the resulting solution was stirred for 16 h then concentrated in vacuo. The residue was diluted with H2O and extracted with Et2O. The aqueous layer was acidified using 2N aqueous HCl solution and the white precipitate formed was extracted twice with AcOEt. The combined organic solutions were dried over Na2SO4 and concentrated in vacuo to give 3-methylsulfanyl-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid (A1) (109 mg, 100%) as a white solid. [M+H]+=252.0, RT=2.61 min

1. stirringthe resulting solution was stirred for 16 h
2. concentrationthen concentrated in vacuo
3. additionThe residue was diluted with H2O
4. extractionextracted with Et2O
5. customthe white precipitate formed
6. extractionwas extracted twice with AcOEt
7. dry with materialThe combined organic solutions were dried over Na2SO4
8. concentrationconcentrated in vacuo