HRID919784
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1-Benzyl-3-{[methoxycarbonylmethyl-(toluene-4-sulfonyl)-amino]-methyl}-6-oxo-1,6-dihydro-pyridine-2-carboxylic acid ethyl ester (0.14 g, 0.27 mmol) was dissolved in MeOH (10 mL) and cooled in an ice bath. NaOMe solution (0.2 mL, 0.82 mmol, 25 wt % in MeOH) was added, and the mixture was stirred overnight. The mixture was placed in an ice bath, and 1 M HCl was added until pH was about 3. The resulting mixture was extracted with CH2Cl2. The organic layer was dried over MgSO4 and concentrated. The residue was chromatographed (10-90% EtOAc/hexanes+2% AcOH) to give 76 mg of the title compound. MS: (−) m/z 311.30 (M+1).
WORKUP
后处理
- temperaturecooled in an ice bath
- customThe mixture was placed in an ice bath
- extractionThe resulting mixture was extracted with CH2Cl2
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated
- customThe residue was chromatographed (10-90% EtOAc/hexanes+2% AcOH)