反应详情

To 500 ml of water are added 50.0 g of 2-amino-5-n-propylbenzenesulfonic acid and 6.28 g of sodium carbonate and the mixture was dissolved by heating. To the solution was added 88.13 g of bis(2-chloroethyl)amine hydrochloride and the mixture was refluxed by heating for 3 hours, And then, a suspension containing 26.25 g of sodium carbonate suspended in 63 ml of water was added thereto, and the mixture was refluxed by heating for 12 hours. The reaction mixture was condensed under reduced pressure, extracted with methyl alcohol and then methyl alcohol was removed under reduced pressure. To the residue was added 200 ml of water, and after a pH of the mixture was adjusted to about 8.0 with sodium carbonate, 500 ml of chloroform was added thereto and the mixture was stirred. Precipitated crystals were collected by filtration, washed with chloroform and dried to give 44.83 g (yield: 67.9%) of the above title product.

1. dissolutionthe mixture was dissolved
2. temperatureby heating
3. temperaturethe mixture was refluxed
4. temperatureby heating for 3 hours
5. additionwas added
6. temperaturethe mixture was refluxed
7. temperatureby heating for 12 hours
8. customcondensed under reduced pressure
9. extractionextracted with methyl alcohol
10. custommethyl alcohol was removed under reduced pressure
11. additionTo the residue was added 200 ml of water
12. additionwas added
13. customPrecipitated crystals
14. filtrationwere collected by filtration
15. washwashed with chloroform
16. customdried