HRID731643

反应详情

EQUATION

反应方程式

HRID 731643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of [2-(5-methyl-3-phenyl-isoxazol-4-yl)-imidazo[1,2-a]pyridin-7-yl]-carbamic acid tert-butyl ester (1.0 g, 2.56 mmol) in hydrochloric acid (4 M in dioxane, 29 mL) was stirred at room temperature for 6 h. The precipitate was then filtered off and dissolved in a dilute solution of sodium hydrogen carbonate and then extracted with ethyl acetate. The organic layer was then washed with brine and then dried over sodium sulphate and evaporated to leave a brown foam. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 25:75) afforded the title compound (477 mg, 64%) which was obtained as a light brown foam. MS: m/e=291.1 [M+H]+.

WORKUP

后处理

  1. filtrationThe precipitate was then filtered off
  2. dissolutiondissolved in a dilute solution of sodium hydrogen carbonate
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was then washed with brine
  5. dry with materialdried over sodium sulphate
  6. customevaporated
  7. customto leave a brown foam
  8. customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 25:75)