反应详情

40 ml of acetonitrile was added to 5.0 g of 4-(3-phenoxycarbonylaminophenyl)-3-methyl-5-mercaptotriazole (6) prepared in Step 1-5. 8.2 g of triethylamine was added to the system. 4.1 g of oxalic acid salt of diethyl 3-aminopropylphosphonate (8) prepared in Step 1-7 was added to the system. The system was then allowed to undergo reaction at a temperature of 50° C. over 4 hours. After the completion of the reaction, the solvent was distilled off under reduced pressure. 100 ml of water was added to the residue to deposit 62 g of a crystal of 4-[3-{3-(3-diethylphosphonopropyl)ureido}phenyl]-3-methyl-5-mercaptotriazole (9). (Yield: 94%; m.p. 128° C.)

1. customreaction at a temperature of 50° C. over 4 hours
2. customAfter the completion of the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. addition100 ml of water was added to the residue