反应详情

温度

25 °C

71 Parts of 2,4-dinitro-N-methylaniline and 53 parts of sodium hydrogen carbonate are stirred in 144 parts of methanol. The yellow suspension is heated in the course of 20 minutes to 40° C. Simultaneously, 81.9 parts of 60% sodium sulphide are dissolved in 144 parts of water of approx. 40° C and 1.2 parts of 30% sodium hydroxide solution are added to the resultant solution. The turbid yellow solution is filtered. The clear yellow filtrate is added dropwise in the course of 2 hours to the suspension of 2,4-dinitro-N-methylaniline. An exothermic reaction occurs during the dropwise addition. The contents of the flask turn dark in colour. The new suspension is heated in the course of 1 hour to 70° C and stirred for 15 minutes at this temperature (reflux). Then 144 parts of methanol are distilled off. The residue is cooled to 25° C and 50 parts of ice are added. After suction filtration at 8° C, the filter cake is washed three times with 160 parts of water and dried in vacuo at 60° C, affording 56.8 parts of 2-amino-4-nitro-N-methylaniline (94.4% of theory). The melting point of the product is 177°-178° C.

1. temperatureThe yellow suspension is heated in the course of 20 minutes to 40° C
2. filtrationThe turbid yellow solution is filtered
3. additionThe clear yellow filtrate is added dropwise in the course of 2 hours to the suspension of 2,4-dinitro-N-methylaniline
4. customAn exothermic reaction
5. additionoccurs during the dropwise addition
6. temperatureThe new suspension is heated in the course of 1 hour to 70° C
7. distillationThen 144 parts of methanol are distilled off
8. addition50 parts of ice are added
9. filtrationAfter suction filtration at 8° C
10. washthe filter cake is washed three times with 160 parts of water
11. customdried in vacuo at 60° C