HRID60736
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
To a solution of (S)-2-aminopentanedioic acid (100 g, 680 mmol) in H2O (500 mL) was added HCl (140 mL, 1.6 mol) and then NaNO2 (70.4 g, 1.02 mol) in H2O (100 mL) was added slowly at −5° C.-0° C., and the reaction mixture was stirred at room temperature for 24 hours. The solvent was concentrated in vacuo below 50° C. The residue was suspended in EtOAc (500 mL) and filtered. The filtrate was dried over Na2SO4 and concentrated in vacuo to afford 56 g crude product of (2S)-5-oxotetrahydrofuran-2-carboxylic acid (compound 28a) as yellow oil, which was used in next step without further purification.
WORKUP
后处理
- concentrationThe solvent was concentrated in vacuo below 50° C
- filtrationfiltered
- dry with materialThe filtrate was dried over Na2SO4
- concentrationconcentrated in vacuo