HCID 22155118, compound → HCID 22155112, compound

Participants

Reaction Steps

2-Methyl-5,6-dimethylthiobenzothiazole was prepared by combining N-acetyl-2,4,5-trimethylthioaniline (20 g , 0.073 mol) and phosphoryl chloride (40 mL) and heating the mixture on a steam bath for 10 min. During this time the reaction mixture solidified. The solid was collected, washed with ether and dried, affording 27 g of the hydrochloride salt. The free base was prepared by dissolving the salt in a mixture of 300 mL of ether and 300 mL of methanol and adding 35 mL of triethylamine. The solvents were evaporated, the solid was collected, slurried with distilled water, collected, and washed with warm water and dried (16 g, 91% yield), mp 79-81° C.

Provenance & Evidence