反应详情

温度

25 °C

8.8 Ml. of 2N sodium hydroxide are added while stirring at 25° C. to a mixture of 5.2 g. of 3-dimethylcarbamoyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonamide in 180 ml. of acetone, during which the solid material first dissolves and then a new crystalline precipitate immediately results. 2.26 Ml. of cyclohexylisocyanate are then added thereto while cooling externally with ice and stirring, whereupon the solid material passes completely into solution and then a crystalline precipitate soon reappears. The mixture is subsequently stirred for 16 hours at 25° C., then diluted with 350 ml. of water, acidified to pH 2 with 3N hydrochloric acid and finally extracted twice with 500 ml. of chloroform each time. The chloroform extracts are dried over sodium sulfate and evaporated in vacuo at 60° C. The residue is dissolved in 25 ml. of acetone and crystallized by trituration. There is obtained 1-cyclohexyl-3-[(3-dimethylcarbamoyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)sulfonyl]urea, m.p. 113° C. (with decomposition).

1. customa new crystalline precipitate immediately results
2. temperaturewhile cooling externally with ice
3. stirringstirring, whereupon the solid material passes completely into solution
4. stirringThe mixture is subsequently stirred for 16 hours at 25° C.
5. additiondiluted with 350 ml
6. extractionfinally extracted twice with 500 ml
7. dry with materialThe chloroform extracts are dried over sodium sulfate
8. customevaporated in vacuo at 60° C
9. dissolutionThe residue is dissolved in 25 ml
10. customof acetone and crystallized by trituration