Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Bromoethyl ethyl ether | HCID 61141 | — |
| Reactant | HCID 56947596 | HCID 56947596 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66835837 | HCID 66835837 | — |
Reaction Steps
A solution of 2-[(3-iodophenyl)(1-methylpiperidin-4-yloxy)methyl]-1H-benzimidazole (example 51, 260 mg) in anhydrous acetonitrile (10 mL) is treated with 60% sodium hydride (47 mg) for 30 min at room temperature. 1-Bromo-2-ethoxyethane (84 μL) is then introduced. After warming at 60° C. for 8 h, dilution with water and extraction with diethylether, the organic phase is dried over magnesium sulfate and concentrated under reduced pressure. The residue is purified by chromatography over silica gel (gradient dichloromethane/methanol/ammonia from 98/2/0.5 to 95/5/0.5) to afford the pure base that is then converted into its dioxalate salt in acetone to give 1-(2-ethoxyethyl)-2-[(3-iodophenyl)(1-methylpiperidin-4-yloxy)methyl]-1H-benzimidazole, dioxalate, melting at 88° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09029357B2 |
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| Source dataset | uspto-grants-2015_05 |
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| ORD ID | ord-d0a69bf86d0b4781a4ae199ad6a95aaa |
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| Source note | uspto-grants-2015_05 |
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