[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:10]=[C:9]([S:11][CH3:12])[N:8]([CH3:13])[N:7]=1.O.O.Cl[Sn]Cl.[OH-].[Na+]>O.Cl>[NH:5]([C:6]1[CH:10]=[C:9]([S:11][CH3:12])[N:8]([CH3:13])[N:7]=1)[NH2:1]
1.1 g (15.8 mmol) sodium nitrite in 4 ml water was added dropwise to 1.9 g (13.1 mmol) 3-amino-1-methyl-5-methylmercaptopyrazole in 28 ml concentrated hydrochloric acid at 0° C. and the mixture stirred for 2 hours at 0° C. Then, at -30° C., a solution of 7.4 g (32.8 mmol) SnCl2.2H2O in 5.5 ml concentrated hydrochloric acid was added dropwise and the mixture stirred for 3 hours at this temperature. The reaction mixture was then made basic with 32% caustic soda and extracted with methylene chloride. The organic phase was dried over sodium sulfate and concentrated. 2.0 g of product was obtained which was used without further purification.
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