Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Reactant | HCID 178497326 | HCID 178497326 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22402944 | HCID 22402944 | 45.8% |
Reaction Steps
Sodium hydride (0.750 g, 80% oil dispersion, 25.0 mmol) is added, in portions, to a solution of dimethyl 2-methyl-4,5-benzimidazoledicarboxylate (6.07 g, 24.6 mmol) in dry dimethylformamide at 0° C. with stirring. After evolution of hydrogen ceases, benzyl bromide (2.93 mL, 24.6 mmol) is added to the reaction mixture and stirring is continued for 16 hours. The reaction mixture is concentrated in vacuo and the resultant residue is dispersed in methylene chloride and water. The phases are separated and the aqueous phase is extracted with methylene chloride. The organic phases are combined, dried and concentrated in vacuo to afford a solid residue. Recrystallization of the solid from ethyl acetate affords the title product as an off-white powder (3.81 g, 45.0%), mp 192°-195° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05516751 |
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| Source dataset | uspto-grants-1996_05 |
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| ORD ID | ord-b5c599ec5e344c8ca326da5aedbdb75c |
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| Source note | uspto-grants-1996_05 |
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