HRID542827

反应详情

EQUATION

反应方程式

HRID 542827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of acetic anhydride (0.8 ml) and formic acid (0.4 ml) was stirred at 50°-60° for 2 hours, then cooled to ambient temperature. 1-(4-Fluoro-2-methylaminophenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanone (1.03 g) was added. The mixture was stirred at ambient temperature for 5 hours, then kept at this temperature for 16 hours. The mixture was triturated under light petroleum to give a solid product. This product was extracted with boiling ethyl acetate (100 ml) and the extract cooled to give a solid product which was recrystallised from industrial methylated spirit to give the novel compound 7-fluoro-1-methyl-3-(1-methyl-1H-tetrazol-5-yl)-4-quinolone, m.p. 264°-267°, identical to the product of Example 2(d).

WORKUP

后处理

  1. stirringThe mixture was stirred at ambient temperature for 5 hours
  2. waitkept at this temperature for 16 hours
  3. customThe mixture was triturated under light petroleum
  4. customto give a solid product
  5. extractionThis product was extracted with boiling ethyl acetate (100 ml)
  6. temperaturethe extract cooled
  7. customto give a solid product which
  8. customwas recrystallised from industrial methylated spirit