HRID358667

反应详情

EQUATION

反应方程式

HRID 358667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Fluoro-3-hydroxy-1 -methyl-4-quinolone (4.5 g) was added to a solution of sodium hydroxide (12 g) in water (56 ml) and the mixture stirred at 0 to 5° with ice/water cooling. Methanesulphonyl chloride (4 ml) was added over a period of 1 5 minutes followed by aqueous sodium hydroxide (5M, 3 ml). The resultant solid was collected by filtration, washed with water (2×20 ml), and crystallised from industrial methylated spirit (220 ml) to give the novel compound 7-fluoro-]-methyl-4-oxo-1,4-dihydroquinol-3-yl methanesulphonate, m.p. 212°-213°.

WORKUP

后处理

  1. filtrationThe resultant solid was collected by filtration
  2. washwashed with water (2×20 ml)
  3. customcrystallised from industrial methylated spirit (220 ml)