Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Hexamethylphosphoramide | HCID 12679 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86750225 | HCID 86750225 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86750226 | HCID 86750226 | — |
Reaction Steps
To a suspension of sodium hydride (6.1 mg) in tetrahydrofuran (1.5 ml) was added a solution of the compound prepared in example 15 (70 mg) in tetrahydrofuran (3 ml) under an atmosphere of argon. The mixture was stirred for 30 min at room temperature. To the mixture were successively added methyl iodide (261 mg) and hexamethylphosphoramide (1 ml), After stirred for 2 h at room temperature, the mixture was diluted with ethyl acetate and water. The mixture was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (ethyl acetate:hexane =2:3) to give the title compound (27 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05596009 |
|---|
| Source dataset | uspto-grants-1997_01 |
|---|
| ORD ID | ord-0a40a64eb5fd4534b8890b7eadef87df |
|---|
| Source note | uspto-grants-1997_01 |
|---|