HRID1708539

反应详情

EQUATION

反应方程式

HRID 1708539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated at 60°~65° C. for one hour
  2. customto give a solid
  3. filtrationThe solid was filtered
  4. dissolutiondissolved in dichloromethane (100 ml)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customto give a residue
  8. customThe residue was triturated with n-hexane