HRID1708548

反应详情

EQUATION

反应方程式

HRID 1708548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 1-(ethoxymethyl)methylamino-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate (200 mg) in dry acetonitrile (2.0 ml) was added trichloromethylsilane (65.8 μl) under ice -cooling and the mixture was stirred for 30 minutes, and then for 10 minutes at room temperature. To the reaction mixture was added diisopropyl ether (10 ml), which was then stirred for 15 minutes at ambient temperature. The precipitate was collected by filtration and washed with diisopropyl ether and dried in vacuo over phosphorus pentaoxide to give ethyl 1-(chloromethyl)methylamino-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate (145 mg).

WORKUP

后处理

  1. waitfor 10 minutes at room temperature
  2. stirringwas then stirred for 15 minutes at ambient temperature
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with diisopropyl ether
  5. dry with materialdried in vacuo over phosphorus pentaoxide