反应详情

To a stirred suspension of 4-bromo-2,6-dinitroaniline (110 g, 420 mmol) in HCl conc (2200 mL) at −20° C. was added tin(II)chloride dihydrate (568 g, 2519 mmol, 6 eq) in one portion under cooling. After stirring overnight ar rt, water (1000 mL) was added to the suspension, and the pH was adjusted to 10 using sodium hydroxide (50% aqueous solution). After extraction with ethyl acetate (3×2000 mL), the organic phase was washed with saturated sodium chloride solution, dried over sodium sulphate and evaporated in vaccuo to yield 81.5 g 5-bromobenzene-1,2,3-triamine (96.1%).

1. temperatureunder cooling
2. extractionAfter extraction with ethyl acetate (3×2000 mL)
3. washthe organic phase was washed with saturated sodium chloride solution
4. dry with materialdried over sodium sulphate
5. customevaporated in vaccuo