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4-Amino-2,6-dibromo-3-nitropyridine synthesis

8synthesis methods
-

Yield:848470-14-4 91%

Reaction Conditions:

Stage #1: 4-amino-2,6-dibromopyridinewith sulfuric acid;nitric acid at 0 - 20; for 0.75 h;
Stage #2: with sulfuric acid at 100; for 0.75 h;

Steps:

Q

Q. 2, 6-Dibromo-3-nitro-pyridin-4-ylamine A solution of 9.5 G (37.7 MMOL) 2, 6-dibromo-pyridin-4-ylamine in 15.3 ml concentrated sulphuric acid was cooled to 0 C and CONC. nitric acid (6.1 ml) was cautiously added. The mixture was cooled to room temperature and stirred for 45 min.. The reaction was poured into ice-water (150 ML), the precipitate filtered off and washed with ethyl acetate. 8.2 G (27.6 MMOL) of the yellow solid were carefully added to 82 ml conc. sulphuric acid and the reaction. heated at 100 C for 45 min.. The reaction mixture was cooled to room temperature and poured into ice. The precipitate was collected by filtration and dried in vacuo at 40 C to afford 7.3 G (91 %) of the title compound as a yellow solid. m. p. 140 C.

References:

WO2005/26164,2005,A1 Location in patent:Page/Page column 44

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