HRID1797307
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
Compound 148 (0.20 g, 0.56 mmol) was dissolved in dry DCM (1 mL) in oven dried glass ware under an argon atmosphere. Diethylphosphonoacetic acid (0.09 mL, 0.56 mmol) was added followed by dropwise addition of dicyclohexylcarbodiimide (0.13 g, 0.61 mmol dissolved in 1 mL dry DCM). The suspension was stirred at room temperature for 7 h after which it was filtered. The filtrate was diluted with 5 mL DCM and washed with 10% aqueous NaHCO3, H2O and brine. The organic phase was dried (MgSO4), filtered and concentrated in vacuo. The crude product was purified by flash chromatography using EtOAc as the eluent to afford the title compound as a slightly coloured oil.
WORKUP
后处理
- customdried glass ware under an argon atmosphere
- filtrationwas filtered
- additionThe filtrate was diluted with 5 mL DCM
- washwashed with 10% aqueous NaHCO3, H2O and brine
- dry with materialThe organic phase was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude product was purified by flash chromatography