HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 22101278, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 22101282 | HCID 22101282 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22101278 | HCID 22101278 | — |
Reaction Steps
The N-(1-hydroxy-2,3-dihydro-1H-phenalen-2-yl)acetamide obtained is stage C of Example 1 (1 mmol, 290 mg) is dissolved in 10 cm3 of anhydrous DMF. Under an inert atmosphere, NaH (1 mmol, 0.05 g of 60% in oil suspension) and then methyl iodide (0.09 cm3, 1.2 eq) are added in the reaction mixture. Stirring is maintained at ambiant temperature for 4h30 and the solvent is evaporated. The residue is taken up in CH2 Cl2 and the solution is flitrated. The filtrate is evaporated and purified by chromatography on silica gel (particle size 60-200 μm); eluent: CH2Cl2 : MeOH 99 :-1 v/v. The title product is isolated. This is and amorphous product, which is a diastereoisomer mixture.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05712312 |
| Source dataset | uspto-grants-1998_01 |
| ORD ID | ord-20d9a9900ddb48ff9621b67c97711d5f |
| Source note | uspto-grants-1998_01 |