2-Fluoro-6-methoxypyridin-4-amine synthesis

Yield:1227586-58-4 58.58%

Reaction Conditions:

Stage #1: sodium methylatewith methanol in 1,4-dioxane at 0 - 30; for 1 h;
Stage #2: 4-amino-2,6-difluoropyridine in 1,4-dioxane at 0 - 30; for 17.33 h;Temperature;Time;

Steps:

1.1; 2.1 A method for synthesizing 4-chloro-6-fluoropyridin-2-ol, which includes the following steps:

(1) At a low temperature of 0°C, use 50mL of dioxane as a solvent, add 2g of sodium methoxide and 6g of methanol, mix well, heat up to 30°C, react for 1h, and cool to 0°C.Add 5g of compound A, divide the compound A according to the same mass, and add it in 2 times, each time with an interval of 10 minutes, heating to 30°C, stirring for 17h, TLC detection, the reaction of the raw materials is complete, cooling to 0°C, adding 80mL of water dropwise Extract with ethyl acetate (120 mL *3), concentrate the organic phase, mix with silica gel and pass through the column to obtain 3.2 g of white solid, compound B, with a yield of 58.58% and a purity of 98.2%

References:

CN111606845,2020,A Location in patent:Paragraph 0014; 0016