HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluidine → (RS)-1-Benzyl-3-hydroxy-3-((4-methylphenyl)aminocarbonylmethyl)indolin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluidine | HCID 7813 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | 1-Benzyl-3-(ethoxycarbonylmethyl)-3-hydroxyindolin-2-one | HCID 264548 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (RS)-1-Benzyl-3-hydroxy-3-((4-methylphenyl)aminocarbonylmethyl)indolin-2-one | HCID 22013019 | 45.3% |
Reaction Steps
To a solution of 0.254 g of p-toluidine in 10 ml of dry tetrahydrofuran was added dropwise 1.3 ml of a 1.59M hexane solution of n-butyl lithium at -78° C. under a nitrogen atmosphere, followed by stirring at that temperature for 10 minutes. To the mixture was added a solution of 0.299 g of 1-benzyl-3-(ethoxycarbonylmethyl)-3-hydroxyindolin-2-one in 5 ml of dry tetrahydrofuran at -78° C., followed by stirring at that temperature for 30 minutes. Water was added to the reaction mixture, and the product was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1) to give 0.161 g (44%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06031111 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-66f1d02f545e41f5aac42d1a64fe4a14 |
| Source note | uspto-grants-2000_02 |