HRID1259360

反应详情

EQUATION

反应方程式

HRID 1259360 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triflic anhydride (2.8 g, 0.010 mol) was added to a stirred solution of 1-benzyl-7-hydroxy-6-methyl-8-nitro-2,3-dihydro-1H-imidazo[1,2-a]pyridin-5-one (2 g, 0.007 mol) and TEA (1.34 g, 0.013 mol) in DCM (40 mL) at −78° C. The resulting mixture was stirred at room temperature for 4 hours. The reaction mixture was monitored by TLC (100% ethyl acetate). The reaction mixture was partitioned between DCM and water. The organic layer was washed with NaHCO3 solution, brine solution, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (30% ethylacetate in hexane) afforded 2.5 g of the product (89% yield).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between DCM and water
  2. washThe organic layer was washed with NaHCO3 solution, brine solution
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customPurification by column chromatography on silica gel (30% ethylacetate in hexane)