HRID1622063
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 the obtained approximately 1.4 g dimethyl 2,2′-(hex-5-ynylazanediyl)diacetate was added 20 mL THF and 20 mL of 2 M KOH. The mixture was stirred overnight and monitored by TLC. The organic layer was separated, and the aqueous layer was quenched by addition of 20 mL of 2 M HCl. The solvent (H2O) was removed by rotary evaporation, and the resulting solid was dissolved into acetonitrile (ACN). The insoluble KCl salt was filtered, and the filtrate was concentrated by rotary evaporation. The final product of free acid was obtained as a greasy, transparent oil. Yield was quantitative. ESI-MS: [M+H]+ m/z 214.1.
WORKUP
后处理
- customThe organic layer was separated
- customthe aqueous layer was quenched by addition of 20 mL of 2 M HCl
- customThe solvent (H2O) was removed by rotary evaporation
- dissolutionthe resulting solid was dissolved into acetonitrile (ACN)
- filtrationThe insoluble KCl salt was filtered
- concentrationthe filtrate was concentrated by rotary evaporation