反应 #51668

ord-0668754525574672803c0c12c2c5681b

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to reflux
  2. 2
    温度heated at this temperature for 3 h
  3. 3
    温度At the end of 3 h, the reaction was cooled
  4. 4
    其他evaporated to dryness

实验过程

The 2-chloro-6-methanesulfonylmethyl-phenylamine (2.04 g, 0.019 mole) of Step 4 was suspended in 15 ml trimethyl orthoformate and p-toluenesulfonic acid hydrate (0.21 g) was added. The reaction mixture was brought to reflux and heated at this temperature for 3 h. The reaction was monitored by tlc (3:7 ethyl acetate:hexane, silica gel) which showed the appearance of a new slightly less polar spot. At the end of 3 h, the reaction was cooled and evaporated to dryness to afford N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-formimidic acid methyl ester.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06852726B2uspto-grants-2005_02