HRID1259384
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
Triflic anhydride (2.78 g, 9.9 mmol) was added dropwise to a stirred solution of 7-hydroxy-6-methyl-8-nitro-2,3-dihydro-oxazolo[3,2-a]pyridin-5-one (1.5 g, 7.0 mmol) and TEA (1.42 g, 14.060 mmol) in DCM (30 mL) at −78° C. over a period of 1 hour. The resulting mixture was stirred at room temperature for 5 hours. The reaction mixture was monitored by TLC (50% ethylacetate in hexane). The reaction mixture was partitioned between DCM and water. The organic layer was washed with water, brine solution, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (50% ethylacetate in hexane) afforded 0.5 g of the product (20.6% yield).
WORKUP
后处理
- customThe reaction mixture was partitioned between DCM and water
- washThe organic layer was washed with water, brine solution
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customPurification by column chromatography on silica gel (50% ethylacetate in hexane)