HRID1257336
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
A solution (4 mL) of the crude compound (290 mg, 0.88 mmol) obtained in Example 26a in tetrahydrofuran was cooled in an ice bath, triethylamine (0.16 mL, 1.14 mmol) and methoxyacetylchloride (115 mg, 1.06 mmol) were added, and the mixture was stirred at room temperature overnight. After confirmation of the termination of the reaction by TLC, the resulting salt was removed. The solvent was evaporated under reduced pressure. The resulting crude title compound was purified by column chromatography (hexane-hexane/ethyl acetate=30/70-ethyl acetate) to give the title compound (339 mg, 96% in 2 steps) as a colorless oil.
WORKUP
后处理
- customAfter confirmation of the termination of the reaction by TLC
- customthe resulting salt was removed
- customThe solvent was evaporated under reduced pressure
- customThe resulting crude title compound was purified by column chromatography (hexane-hexane/ethyl acetate=30/70-ethyl acetate)