Methane → HCID 20472817, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 164 parts of 2-iminobenzothiazoline, 150 parts of sodium hydroxide and 300 parts of ethyleneglycol is stirred for 6 hours at 130°-140° C., subsequently cooled to 80° C., and introduced with agitation into 3000 parts of icewater. After further agitation for 30 minutes, 5 parts of active charcoal are added, the solution is stirred for a further 15 minutes and then filtered. The pH of the filtrate is adjusted to 5-6 by means of 10% aqueous hydrochloric acid, and the precipitated N-methyl-N-(2-mercaptophenyl)-urea is isolated by filtration. The moist product is immediately introduced into 700 parts of a 10% aqueous hydrochloric acid and heated for 15 minutes with agitation at 90° C. The precipitating 3-methyl-2(3H)-benzothiazolone of the formula ##STR4## is isolated by filtration after cooling the acidic batch, washed with water and dried. 150 Parts of an analytically pure product are obtained; this corresponds to a yield of 90.9% of theory, relative to 2-iminobenzothiazoline, melting point 73°-75° C.

Provenance & Evidence