HRID338810

反应详情

EQUATION

反应方程式

HRID 338810 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a methanol solvent, a solution including Compound 97b (1.0 eq.) and 2-aminothiophenol (1.0 eq.) was stirred at room temperature for 22 hours. After methanol was evaporated, the residual was purified by silica gel column chromatography using hexane and ethyl acetate (14:1) as a developer. The obtained product was dissolved with 1,4-dioxane, and then, 1 N NaOH (1.5 eq.) was added thereto. The reaction mixture was stirred at room temperature for 17 hours, and 1,4-dioxane was evaporated. The reaction mixture was stirred at room temperature for 17 hours, and 1,4-dioxane was evaporated therefrom. The residual was distributed between ethyl acetate and water, an aqueous layer was acidified with 6 N HCl. The produced precipitate was filtered and washed with water to obtain Compound 120.

WORKUP

后处理

  1. customAfter methanol was evaporated
  2. customthe residual was purified by silica gel column chromatography
  3. dissolutionThe obtained product was dissolved with 1,4-dioxane
  4. stirringThe reaction mixture was stirred at room temperature for 17 hours
  5. custom1,4-dioxane was evaporated
  6. stirringThe reaction mixture was stirred at room temperature for 17 hours
  7. custom1,4-dioxane was evaporated
  8. filtrationThe produced precipitate was filtered
  9. washwashed with water