HRID986009

反应详情

EQUATION

反应方程式

HRID 986009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-[1H]-quinolone (2.0 g) and silver sulphate (2.14 g) in concentrated sulphuric acid (15.0 cm3) was stirred at room temperature during the addition of iodine (3.5 g). After heating at 50° for 24 hours the mixture was poured onto ice, the solution was neutralised with solid sodium carbonate and the solid was filtered off. This material was chromatographed on silica (Merck "MK 60.9385") eluting with chloroform to affford a residue which was recrystallised from methanol to give 6-iodo-2-[1H]-quinolone, m.p. 261°, (0.8 g).

WORKUP

后处理

  1. temperatureAfter heating at 50° for 24 hours the mixture
  2. additionwas poured onto ice
  3. filtrationthe solid was filtered off
  4. customThis material was chromatographed on silica (Merck "MK 60.9385")
  5. washeluting with chloroform
  6. customwas recrystallised from methanol