HRID1708539
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
A suspension of ethyl 2-(2,3,4,5-tetrafluorobenzoyl)-3-(2-tert-butoxycarbonyl-2-methylhydrazino)acrylate (10.50 g)and potassium carbonate (3.80 g)in dimethylformamide (31.5 ml)was heated at 60°~65° C. for one hour. The mixture was poured into ice-water (300 ml) to give a solid. The solid was filtered , dissolved in dichloromethane (100 ml), dried over magnesium sulfate, and concentrated under reduced pressure to give a residue. The residue was triturated with n-hexane to give ethyl 1-(N-tert-butoxycarbonyl-N-methylamino)-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate (9.25 g).
WORKUP
后处理
- temperaturewas heated at 60°~65° C. for one hour
- customto give a solid
- filtrationThe solid was filtered
- dissolutiondissolved in dichloromethane (100 ml)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give a residue
- customThe residue was triturated with n-hexane