HRID2241997
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
To a solution of tert-butyl 4-[5-(trifluoromethyl)-8-quinolinyl]-1-piperazine-carboxylate (Step 2, 0.85 g) in 5 mL dioxane was added 5 mL of 4 N HCl/dioxane. The mixture was stirred at room temperature overnight. The reaction was concentrated on a rotary evaporator, dissolved in water, neutralized with aqueous sodium hydroxide and extracted with CH2Cl2 The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated on a rotary evaporator to give 0.65 g of the desired product as an off-white solid; MP. 155-157° C.; MS (ES) m/z (relative intensity): 282 (M+H)+ (100).
WORKUP
后处理
- concentrationThe reaction was concentrated on a rotary evaporator
- dissolutiondissolved in water
- extractionextracted with CH2Cl2 The combined organic layers
- dry with materialwere dried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated on a rotary evaporator