HRID1259417

反应详情

EQUATION

反应方程式

HRID 1259417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Triflic anhydride (3.4 g, 12.06 mmol) was added to a stirred solution of 7-hydroxy-6-methyl-8-nitro-2,3-dihydro-thiazolo[3,2-a]pyridin-5-one (2.5 g, 10.96 mmol) and TEA (2.3 mL, 16.44 mmol) in DCM (20 mL) at −70° C. The resulting mixture was stirred at −70° C. to −50° C. for 2 hours. The reaction mixture was monitored by TLC (50% ethylacetate in hexane). The reaction mixture was diluted DCM and quenched with bicarbonate solution. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (30% ethylacetate in hexane) afforded 0.9 g of the product (38% yield).

WORKUP

后处理

  1. customquenched with bicarbonate solution
  2. washThe organic layer was washed with brine solution
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customPurification by column chromatography on silica gel (30% ethylacetate in hexane)