反应详情

A solution of compound 33-1 (29.0 mg, 0.059 mmol) in MeOH (6 mL) was added to 5% aqueous LiOH (3 mL) and the mixture was stirred at rt for 20 h. The mixture was then diluted with water (2 mL), evaporated to ½ of the initial volume and acidified with 5% aqueous HCl. The solution was extracted with EtOAc (3 mL then 1 mL, twice). The organic layers were combined, washed with water (three times, 1 mL) and evaporated to dryness in vacuo. The resulting oily residue was dissolved in DMSO (1.0 mL), filtered and purified by reverse-phase HPLC to give the title compound as off-white solid. LR-MS (API-ES): calculated for C23H15ClN2O3S 434.1, observed m/e 435.0 (M+H)+ (Rt 2.96 min).

1. customevaporated
2. extractionThe solution was extracted with EtOAc (3 mL
3. washwashed with water (three times, 1 mL)
4. customevaporated to dryness in vacuo
5. dissolutionThe resulting oily residue was dissolved in DMSO (1.0 mL)
6. filtrationfiltered
7. custompurified by reverse-phase HPLC