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
2.7 g of tert-butyl ester of 4-[5-(1,4-dioxa-8-aza-spiro[4.5]dec-8-yl)-pyridin-2-yl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid is put in 30 ml of dioxane, then 22.37 ml of 4N HCl in dioxane is added. The reaction mixture is stirred for 48 h in a closed environment at room temperature. After concentration to dryness, the reaction mixture is diluted with 200 ml of a saturated aqueous solution of sodium hydrogen carbonate and extracted twice with 200 ml of dichloromethane. The resultant organic phases are combined, washed with 100 ml of a saturated aqueous solution of sodium hydrogen carbonate, and with 100 ml of a saturated aqueous solution of sodium chloride, dried over MgSO4 and concentrated to dryness. 2.1 g of 1-[5-(1,4-dioxa-8-aza-spiro[4.5]dec-8-yl)-pyridin-2-yl]-1,2,3,4-tetrahydroquinoxaline is obtained.
WORKUP
后处理
- concentrationAfter concentration to dryness
- additionthe reaction mixture is diluted with 200 ml of a saturated aqueous solution of sodium hydrogen carbonate
- extractionextracted twice with 200 ml of dichloromethane
- washwashed with 100 ml of a saturated aqueous solution of sodium hydrogen carbonate
- dry with materialwith 100 ml of a saturated aqueous solution of sodium chloride, dried over MgSO4
- concentrationconcentrated to dryness