HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23158256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 5-Bromo-2-(2-hydroxy-2-methylpropyl)-2,3-dihydro-1H-isoindol-1-one | HCID 23158208 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23158256 | HCID 23158256 | — |
Reaction Steps
Under nitrogen atmosphere, 100 mg of 5-bromo-2-(2-hydroxy-2-methyl-propyl)-1-oxo-isoindoline obtained in Example 177-1) was dissolved in tetrahydrofuran, 40 mg of sodium hydride, 0.4 ml of methyl iodide were added and the mixture was heated under reflux for 2 hours. The reaction solution was cooled down to room temperature, water was added, and the products were extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure, and the residues were separated and purified by thin-layer silicagel column chromatography (ethyl acetate) to obtain 7 mg of the above compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902369B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-bcc8016cf37b4092a55c768cb4784529 |
| Source note | uspto-grants-2011_03 |