HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 18665931, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 18944845 | HCID 18944845 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 18665931 | HCID 18665931 | 71% |
Reaction Steps
To a solution of (+)-methyl-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-2-carboxylate (0.9 g, 4.1 mmoles) in anhydrous toluene (20 ml), NaH (0.12 g, 5.1 mmoles) and methyl iodide (0.87 g, 6.1 mmoles) were added with stirring and the mixture was heated at reflux temperature for 2 hours. After the completion of the reaction, the toluene solution was washed with water (2×20 ml), 0.1M HCl (2×20 ml) and saturated NaCl solution (20 ml). The solution was dried over MgSO4 and the solvent was evaporated. Thus there were obtained 0.68 g of the title product, which was recrystallized from a mixture of hexane and diethyl ether. The title product was in the form of white crystals, m.p. 76°-78° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05824652 |
| Source dataset | uspto-grants-1998_10 |
| ORD ID | ord-8bcc95acc2a54548a12b1326606a502e |
| Source note | uspto-grants-1998_10 |