反应详情

温度

75 °C

A mixture of α-cyano-β-(2-nitro-5-methylthiophenyl)acrylamide (8.4 g., 0.032 mole) in acetic acid - N,N-dimethylformamide (110 ml. of 1:1) is heated in a 75° C. bath. Iron powder (2.0g.) is added and the mixture stirred until the internal temperature rose to 95° C. Additional iron powder (6.16 g. total iron added = 0.146 mole) is added in small portions over a 15-minute period. The reaction mixture is stirred for 1 hour following completion of addition and then filtered hot. The iron residue is washed with hot acetic acid and the combined filtrate and wash solution poured into IN hydrochloric acid (200 ml.). The hydrochloride salt which separates is filtered off and dissolved in hot dilute aqueous sodium hydroxide. The yellow solid which separates on cooling is filtered off, washed with isopropyl alcohol and air-dried. Yield = 3.26 g. (44%); M.P. 229°-242° C.

1. customrose to 95° C
2. stirringThe reaction mixture is stirred for 1 hour
3. additioncompletion of addition
4. filtrationfiltered hot
5. washThe iron residue is washed with hot acetic acid
6. washthe combined filtrate and wash solution
7. additionpoured into IN hydrochloric acid (200 ml.)
8. filtrationThe hydrochloride salt which separates is filtered off
9. dissolutiondissolved in hot dilute aqueous sodium hydroxide
10. temperatureon cooling
11. filtrationis filtered off
12. washwashed with isopropyl alcohol
13. customair-dried