HRID1266576
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
(2R)-3-methyl-2-[(2-methylthiobenzthiazol-6-sulfonyl)amino]butanoic acid methylester (0.35 g, 0.9 mmol) was dissolved in THF/H2O (2 mL/2 mL), and added LiOH (0.16 g, 5 equi.). After the reaction soluton was refluxed for 6 hours, the solution was distilled under reduced pressure and treated with 1N HCl. The product was extracted with ethylacetate (10 mL). The separated organic phase was washed with NaCl solution, dried over MgSO4, distilled under reduced pressure and dried under vacuum, to prepare the titled compound, (2R)-3-methyl-2-[(2-methylthiobenzthiazol-6-sulfonyl)amino]butanoic acid (54 mg, 23%).
WORKUP
后处理
- temperatureAfter the reaction soluton was refluxed for 6 hours
- distillationthe solution was distilled under reduced pressure
- additiontreated with 1N HCl
- extractionThe product was extracted with ethylacetate (10 mL)
- washThe separated organic phase was washed with NaCl solution
- dry with materialdried over MgSO4
- distillationdistilled under reduced pressure
- customdried under vacuum
- customto prepare the titled compound, (2R)-3-methyl-2-[(2-methylthiobenzthiazol-6-sulfonyl)amino]butanoic acid (54 mg, 23%)