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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Ethyl (2S,3S)-2,3-dihydroxy-3-[(S)-3-methyl-1-(3-methylbutylcarbamoyl)butylcarbamoyl]propionate (309 mg) obtained in Example 2 was dissolved in methanol. 2N KOH (472 μl) was added to the resultant solution, and the solution was stirred at 0° C. for two hours. Thereafter, the solvent was distilled off under reduced pressure, sodium bicarbonate solution was added to adjust the pH to be about 8, and the aqueous layer was washed with ethyl acetate. Subsequently, the pH was adjusted to about 2 with dilute hydrochloric acid, sodium chloride was added until the solution was saturated, and the aqueous layer was extracted with ethyl acetate. The extracted organic layer was washed with sodium chloride solution and dried with magnesium sulfate, and the solvent was distilled off under reduced pressure, thereby obtaining 264 mg of a target compound. NMR data of the compound were as follows.
WORKUP
后处理
- distillationThereafter, the solvent was distilled off under reduced pressure, sodium bicarbonate solution
- additionwas added
- washthe aqueous layer was washed with ethyl acetate
- additionwas added until the solution
- extractionthe aqueous layer was extracted with ethyl acetate
- washThe extracted organic layer was washed with sodium chloride solution
- dry with materialdried with magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure