Synthesis method of Anilofos

- May 04, 2018-

The alkylation reaction mixes 0.376 mol of p-chloroaniline with 2-bromopropane and heats the mixture for a few hours at a certain temperature. After cooling, add sodium hydroxide solution and stir and stratify. The oil layer is washed to neutrality, the aqueous layer is solvent extracted, and the oil layer is combined. Decolorization of the purple liquid 64g, 4-chloro-N-isopropylaniline, yield 95% to 98%. Or use p-nitrochlorobenzene and acetone, hydrogen at the same time to make 4-chloro-N-isopropylaniline. Or with chloroaniline and isopropanol in the presence of a solid catalyst, at 135 ~ 140 °C, 0.67 ~ 0.7MPa reaction 5h obtained. Chloroacetylation The above-mentioned product, 0.48 mol, a solvent, and chloroacetyl chloride are mixed and heated, and reacted at a certain temperature for several hours. Stir with water, stand for stratification, wash the oil layer, extract the aqueous layer, and combine the oil layers. After desolvation, light red N-chloroacetyl-N-isopropylp-chloroaniline (119 g, yield 98%). It has also been reported that pyridine is used as an acid-binding agent and the reaction is carried out at a relatively low temperature. After the condensation reaction, 0.17 mol of N-chloroacetyl-N-isopropylp-chloroaniline, acid-binding agent, solvent and O,O-dimethyldithiophosphoric acid were mixed, and the reaction was stirred at a certain temperature for several hours. The water elution solution was 63 g of Shafen Phosphorus, with a yield of 88% to 90%.