反应详情

温度

150 °C

A mixture of 1.0 g of 2-amino-5-iodo-3-methylbenzoic acid, 0.45 g of copper cyanide and 10 ml of N,N-dimethylformamide was stirred at 150° C. for 9 hours. The reaction mixture was concentrated under reduced pressure. Into the residue, 20 ml of water and 2 ml of ethylenediamine were poured, and the mixture was stirred at room temperature for 1 hour. After the reaction mixture was filtered, the filtrate was adjusted to around pH 5 by an addition of concentrated hydrochloric acid, and then extracted with ethyl acetate three times. The combined organic layer was dried over sodium sulfate, and concentrated under reduced pressure to obtain 0.40 g of 2-amino-5-cyano-3-methylbenzoic acid of the formula:

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionInto the residue, 20 ml of water and 2 ml of ethylenediamine were poured
3. stirringthe mixture was stirred at room temperature for 1 hour
4. filtrationAfter the reaction mixture was filtered
5. additionthe filtrate was adjusted to around pH 5 by an addition of concentrated hydrochloric acid
6. extractionextracted with ethyl acetate three times
7. dry with materialThe combined organic layer was dried over sodium sulfate
8. concentrationconcentrated under reduced pressure