Methyl iodide → HCID 53255561, compound

Participants

Reaction Steps

In analogous manner to that described in Preparation Example 1 Variant A a), 3g of 2-[3-fluoro-2-nitrophenoxy]ethanol were prepared from 5g of 3-fluoro-2-nitrophenol. 1.4g of the alcohol were then reacted with 7ml methyliodide with the addition of 14ml of 50% sodium hydroxide and 0.1g of the phase transfer catalyst, triethylbenzylammonium chloride. The mixture was stirred at room temperature for 2 hours. 20ml of water was then added and the product extracted into 50ml diethyl ether and the ether layer dried using magnesium sulphate. 0.8g (yield of 53%) of 3-fluoro-2-nitrophenyl (2-methoxyethyl) ether were obtained, after the solvent had been removed by evaporation, as an oil which solidified on standing. 0.8g (54% yield) of 5,7-dimethyl-2-(N-[2-fluoro-6-(2-methoxyethoxy)phenyl]-sulphamoyl)-1,2,4-triazolo[1,5-a]pyrimidine (Compound No. 11) were prepared from the ether via the 2-amino derivative in an analogous procedure to that described in Preparation Example 1, Variant A.

Provenance & Evidence