2-amino-5-chloro-4-methoxybenzonitrile synthesis

Yield:79025-49-3 62%

Reaction Conditions:

with N-chloro-succinimide in tetrahydrofuran at 60; for 16 h;

Steps:

94.1 Step 1. 2-Amino-5-chloro-4-methoxybenzonitrile.

Into a 100-mL round- bottom flask, was placed 2-amino-4-methoxybenzonitrile (2.0 g, 13.50 mmol), tetrahydrofuran (40 mL) and N-chlorosuccinimide (2.7 g, 20.2 mmol). The resulting solution was stirred for 16 hrs at 60 °C. The resulting solution was extracted with ethyl acetate and the organic phases combined. The combined organics were evaporated in vacuo and the residue was purified on a silica gel column with ethyl acetate/petroleum ether (1/3). This resulted in 1.54 g (62%) of 2- amino-5-chloro-4-methoxybenzonitrile as a light red solid.

References:

WO2017/192304,2017,A1 Location in patent:Paragraph 0318