HRID718704
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 tri-methylsulfoxonium iodide (495 mg, 2.25 mmol) in DMSO (4 mL) was added NaH (90 mg, 2.2 mmol) and the resulting mixture was stirred for 30 min. At this time compound 79a (400 mg, 1.87 mmol) was added in one portion and the resulting mixture was stirred overnight. The reaction mixture was then diluted with EtOAc (100 mL), washed with saturated sodium bicarbonate (100 mL) and concentrated in vacuo to obtain a residue which was purified by flash column chromatography on silica gel (0-50% EtOAc-heptane) to afford compound 79b as a white solid. Mass spectrum (LCMS, ESI pos.) Calcd. For C14H13NO2 228.0 (M+H). found 228.2.
WORKUP
后处理
- stirringthe resulting mixture was stirred overnight
- washwashed with saturated sodium bicarbonate (100 mL)
- concentrationconcentrated in vacuo
- customto obtain a residue which
- customwas purified by flash column chromatography on silica gel (0-50% EtOAc-heptane)