HRID231493
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
30 g of 5-amino-N,N-dipropyl-3-benzothiophencarboxamide were dissolved in 250 ml of dry methanol. 15 g of magnesium turnings were added (eventually activated by addition of a few drops of 1,2-dibromoethane). The mixture was stirred at 30°-35° C. for 4 hours with periodically cooling to keep the temperature down. 2 l of a saturated ammonium chloride solution were added and the product extracted with ethyl acetate. The organic phase was separated, washed with water, dried (MgSO4) and the solvent evaporated. Isopropyl ether was added, and by cooling the title compound precipitated and was filtered off. Yield: 20 g. M.P. 100° C.
WORKUP
后处理
- temperaturewith periodically cooling
- extractionthe product extracted with ethyl acetate
- customThe organic phase was separated
- washwashed with water
- dry with materialdried (MgSO4)
- customthe solvent evaporated
- additionIsopropyl ether was added
- temperatureby cooling the title compound
- customprecipitated
- filtrationwas filtered off