反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter methanol was evaporated
- customthe residual was purified by silica gel column chromatography
- dissolutionThe obtained product was dissolved with 1,4-dioxane
- stirringThe reaction mixture was stirred at room temperature for 17 hours
- custom1,4-dioxane was evaporated
- stirringThe reaction mixture was stirred at room temperature for 17 hours
- custom1,4-dioxane was evaporated
- filtrationThe produced precipitate was filtered
- washwashed with water