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温度

0 °C

The diazonium chloride of 2-amino-3-bromo-5-methylbenzoic acid is obtained by running an aqueous sodium nitrite solution (0.013 mol) dropwise at -5° C. onto a solution containing 0.0109 mol of 2-amino-3-bromo-5-methylbenzoic acid, 10 ml of hydrochloric acid, 10 ml of water and 30 ml of acetic acid. The reaction mixture is then stirred at 0° C. for 30 minutes and then poured into a large-volume round-bottomed flask containing 0.013 mol of cuprous chloride in 10 ml of acetic acid. The mixture obtained is brought to 60° C., stirred for 2 hours, and then hydrolysed after cooling by addition of ice. The precipitate obtained is filtered and washed with water. 3-Bromo-2-chloro-5-methylbenzoic acid is obtained: (Yield 58%, M.p. 160° C.).

1. customdropwise at -5° C.
2. additionpoured into a large-volume round-bottomed flask
3. customThe mixture obtained
4. customis brought to 60° C.
5. stirringstirred for 2 hours
6. temperaturehydrolysed after cooling by addition of ice
7. customThe precipitate obtained
8. filtrationis filtered
9. washwashed with water