HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 3,3-Bis(N'-(4-methylphenyl)ureido)indolin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | N-(4-Methylphenyl)urea | HCID 12148 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3,3-Bis(N'-(4-methylphenyl)ureido)indolin-2-one | HCID 9932375 | 36% |
Reaction Steps
To a solution of 12.0 g of anhydrous aluminum chloride in 150 ml of dry tetrahydrofuran were added successively a solution of 5.79 g of isatin-3,3-dimethylacetal in 150 ml of dry tetrahydrofuran and 9.0 g of p-tolylurea at 0° C. under a nitrogen atmosphere, and the mixture was heated under reflux for 40 minutes. Ethyl acetate was added to the reaction mixture, and the mixture was washed twice with an aqueous solution of sodium chloride. The organic layer was dried over anhydrous sodium sulfate, followed by concentration. To the residue was added 150 ml of ethyl ether, and insoluble matter was removed by filtration. The filtrate was concentrated and recrystallized from acetone to yield 4.61 g (36%) of the title compound as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06127544 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-f3bbc4f67eef49649b9195f693799b03 |
| Source note | uspto-grants-2000_10 |