HRID1259391

反应详情

EQUATION

反应方程式

HRID 1259391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Osmium tetra oxide (8 mg, 0.035 mmol), 2,6-lutidine (0.08 g, 0.74 mmol) and sodium periodate (0.3 g, 0.001 mol) were added to a solution of 1-allyl-cyclopropanesulfonic acid [7-(2-fluoro-4-iodo-phenylamino)-6-methyl-5-oxo-2,3-dihydro-5H-oxazolo[3,2-a]pyridin-8-yl]-amide (0.19 g, 0.35 mmol) in dioxane (7 mL) and water (2 mL). The resulting mixture was stirred at room temperature for 5 hours. The reaction was monitored by TLC (5% MeOH in DCM). The reaction mixture was partitioned between ethylacetate and water. The organic layer was washed with water, brine solution, dried over Na2SO4, filtered and the filtrate was concentrated. Purification by column chromatography on silica gel (2% MeOH in DCM) afforded 0.12 g of the product (63% yield). LCMS: m/z=549 (M+1)

WORKUP

后处理

  1. customThe reaction mixture was partitioned between ethylacetate and water
  2. washThe organic layer was washed with water, brine solution
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. customPurification by column chromatography on silica gel (2% MeOH in DCM)