Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 67747621 | HCID 67747621 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21689292 | HCID 21689292 | 97% |
Reaction Steps
In 5 ml of N,N-dimethylformamide was dissolved 200 mg of the compound obtained in Example 9, and 30.4 mg of 60% sodium hydride was added to the solution, followed by stirring for about 1 hour. To the mixture was added 0.48 ml of iodomethane, and the mixture was allowed to react at room temperature for 2 hours. The reaction mixture was extracted with 300 ml of chloroform, and the chloroform layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The residue was freed of the solvent by distillation under reduced pressure, and the resulting viscous brown liquid was purified by silica gel column chromatography (chloroform:methanol=50:1 to 10:1 by volume) to obtain 202 mg (97%) of the titled compound as a pale yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05185347 |
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| Source dataset | uspto-grants-1993_02 |
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| ORD ID | ord-8aecd00c529947d2999c4080b423d6cc |
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| Source note | uspto-grants-1993_02 |
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