Hydrochloric Acid → HCID 136331503, compound

Participants

Reaction Steps

To a solution of N-iso-butyroyl-N-(2-chloro-5- thiazolylmethyl)-S-methyl-N'-nitroisothiourea (560 mg) in dichloromethane (5 ml) was added 40% methylamine-methanol solution (129 mg) dropwise below -11° C. and the mixture was stirred at the same temperature for 1 hour. To the mixture was added 40% methylamine-methanol solution (64 mg) dropwise below -11° C. and the mixture was stirred at the same temperature for 5.5 hours. After addition of 2N hydrochloric acid (10 ml) under ice-cooling, the mixture was extracted with toluene (5 ml). The organic layer was washed with an aqueous saturated sodium bicarbonate solution, dried over MgSO4 and concentrated in vacuo. The residue was dissolved in toluene. Crystallization by addition of n-hexane gave 190 mg of 1-iso-butyroyl-1-(2-chloro-5-thiazolylmethyl)-3-methyl-2-nitroguanidine (Compound No. 34) as a white crystal, m.p. 101°-104° C.

Provenance & Evidence