HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Dimethylaminopyrimidine → 1,3-Dioxo-2-(2,6-dioxo-3-fluoropiperidin-3-yl)isoindoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Dimethylaminopyrimidine | HCID 521717 | — |
| Reactant | Bis-(1H-imidazol-2-YL)-methanone | HCID 5250894 | — |
| Reactant | 4-(1,3-Dioxoisoindolin-2-yl)-4-(ethoxycarbonyl)-4-fluorobutanoic acid | HCID 21847918 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1,3-Dioxo-2-(2,6-dioxo-3-fluoropiperidin-3-yl)isoindoline | HCID 9882050 | — |
Reaction Steps
A mixture of 4-(1,3-dioxoisoindolin-2-yl)-4-(ethoxycarbonyl)-4-fluorobutanoic acid (0.9 g, 2.8 mmol), carbonyl diimidazole (0.46 g, 2.8 mmol) and dimethylaminopyrimidine (0.68 g, 5.6 mmol) in tetrahydrofuran (30 mL) is heated at reflux for 18 hours. The solvent is removed in vacuo and the residue is stirred with methylene chloride (50 mL) for 10 minutes. The organic layer is washed with water and brine (40 mL each) and dried over sodium sulfate. The solvent is removed in vacuo to give 1,3-dioxo-2-(2,6-dioxo-3-fluoropiperidin-3-yl)isoindoline which is further purified by column chromatography.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05874448 |
| Source dataset | uspto-grants-1999_02 |
| ORD ID | ord-87dd17856fa543278461261f0b8735db |
| Source note | uspto-grants-1999_02 |