Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 70113129 | HCID 70113129 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70112767 | HCID 70112767 | — |
Reaction Steps
To a stirred solution of the product from step (vii) (2.0 g) in tetrahydrofuran (20 ml) at 0° C. was added sodium hydride (60% dispersion by wt, 0.22 g). The mixture was stirred at 0° C. for 40 min and treated with methyl iodide (0.35 ml). The mixture was further stirred at 0° C. for 2 hours and room temperature for 24 hours then partitioned between ethyl acetate and water. The organic phase was washed with water and saturated brine, dried (MgSO4) and solvent evaporated. Purification was by chromatography eluting with 10% ethanol in dichloromethane to give the product as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06218376B1 |
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| Source dataset | uspto-grants-2001_04 |
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| ORD ID | ord-61617e274e1141d9bc844b3972df0eb5 |
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| Source note | uspto-grants-2001_04 |
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