1-Chloro-2,4-Dinitrobenzene → 5-Nitro-1,3-benzothiazol-2-amine

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반응 단계

A suspension of 10.13 g of 2,4-dinitrochlorobenzene and 15.2 g of thiourea in 50 ml of sulpholane (tetrahydrothiophene 1,1-dioxide) is stirred at 110° to 120° C. for 12 hours. After cooling, the mixture is thoroughly stirred with 800 ml of water, and the solid is filtered off with suction and washed with water. After drying, 11.2 g of a yellow powder which, according to HPLC analysis (high pressure liquid chromatography), contains 69.5% of 2-amino-5-nitrobenzothiazole (corresponding to 80% of theory) are obtained. Recrystallisation from dimethylformamide raises the melting point to 307° C. (decomposition) (Zhur. Obschei Khim. 30, 1363-6 (1960) reports melting point 308°-309° C., decomposition).

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