preparation of 1-methyl-p-toluenesulfonylmethyl isonitrile_kain industrial additive

background and overview^[1][2]

1-methyl-p-toluenesulfonylmethyl isonitrile is also known as -((1-isocyanoethyl)sulfonyl)-4-toluene; 1-methyl-1-toluenesulfonylmethylisonitrile cyanide; 1-methyl-1-tosylmethylisobutyl ester, benzene, 1-[(1-isocyanoethyl)sulfonyl]-4-methyl-; 1-tosylethylisocyanide; a-tosylethylisocyanide; is a chemical in organic synthesis , especially the synthesis of five-membered organic heterocycles and the widely used intermediates, which have been used in the synthesis of drugs and other fine chemical products. however, the existing preparation method of 1-methyl-p-toluenesulfonylmethylisonitrile has a very low yield. since it is mixed with water, it is generally not recovered. when prepared in large quantities, it increases the cost and pollutes the environment. cheap or low-cost methods should be considered. easily recyclable solvent replacement.

1-methyl-p-toluenesulfonylmethylisonitrile

preparation^[2]

preparation method of 1-methyl-p-toluenesulfonylmethylisonitrile:

step 1: in a reaction kettle equipped with a stirrer, add n-p-toluenesulfonylmethylformamide, dimethylethyl chloride, anhydrous ether and acetonitrile while stirring, and dissolve the stirring suspension cool to -3°c in an ice-salt bath, add dropwise the mixed solution of ethanol and n-ethane, and complete the dropwise addition within 35m at a constant speed, the white suspension gradually turns brown;

step 2: keep the above brown suspension at 0°c and stir for 40 minutes. add ice water while stirring. filter out the dark brown precipitate from the brown suspension. dissolve the dark brown precipitate in butylbenzene at 68°c and add activated carbon. , stir for 10 m and then filter. add petroleum ether to the solution while vortexing. after 30 m, filter out the precipitate with suction and dry it in a vacuum dryer for 7 hours to obtain a light brown colorless solid product.

main reference materials

[1] ding chengrong, zhang chaoyang, wang xiangang, xiao jun, yan yunbing, & zhang guofu. (2012). synthesis of p-toluenesulfonylmethyl isonitrile. pesticides, 51(12), 869-871.

[2] jiang shuyan, zhao yan, & han yuding. (1997). study on reaction conditions for the synthesis of p-toluenesulfonylmethyl isonitrile. shandong chemical industry (2), 16-18.

[3] wang yanan, liu shiwei, li lu, & yu shitao. (2016). synthesis study of p-toluenesulfonylmethylisonitrile. chemical technology, 24(1), 37-40.