Toluene → HCID 12151387, compound

Participants

Reaction Steps

To the mixture of 20 ml of toluene and 10 ml of water, 2.53 g of 4-methoxybenzylisothiourea hydrochloride, 2.03 g of perchloromethylmercaptan and 50 mg of benzyltriethylammonium chloride were added, followed the solution of 1.74 g of sodium hydroxide dissolved to 10 ml of water was added dropwise over a period for 4 hours at about 0° C. After completion of addition, the mixture was stirred at room tempareture for 1 hour. Then, t-butylmethylether was added to the reaction mixture, and extracted. The organic layer was dried by anhydrous sodium salfate. The concentrated residue obtaind was subjected to silica gel column chromatography to obtain 5.38 g of 3-(4-methoxybenzyl)thio-5-chloro-1,2,4-thiadiazole.

Provenance & Evidence