HRID30450

反应详情

EQUATION

反应方程式

HRID 30450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
48 °C

PROCEDURE

实验过程

A 140 liter reactor equipped with mechanical stirrer, condenser and thermometer, was charged with dimethyl sulfoxide (DMSO, 120 L). The DMSO was heated to 55° C. and the reactor was charged with 2-methylpiperazine (8.6 kg). Gatifloxacin acid was charged, in four portions, every 2 hours (3×4=12 Kg). The reaction mixture was stirred at a rate of 110 rpm under nitrogen atmosphere. The temperature was maintained for 24 hours until completion of the reaction. The reaction mixture was cooled to 48° C. and water (24 L) was added at this temperature. The mixture was cooled to 5° C. during 3.5 hours and maintained with stirring for 15 hours at this temperature. The mixture was filtered (suction) and washed with acetonitrile (18 L) to obtain 15.9 Kg of gatifloxacin.

WORKUP

后处理

  1. customA 140 liter reactor equipped with mechanical stirrer, condenser
  2. temperatureThe temperature was maintained for 24 hours until completion of the reaction
  3. temperatureThe mixture was cooled to 5° C. during 3.5 hours
  4. temperaturemaintained
  5. stirringwith stirring for 15 hours at this temperature
  6. filtrationThe mixture was filtered (suction)
  7. washwashed with acetonitrile (18 L)