Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-methyl-2,3-dihydro-1H-1,3-benzodiazol-2-one | HCID 590540 | — |
| Reactant | 1,4-Dichloro-cis-2-butene | HCID 6432115 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59075602 | HCID 59075602 | — |
Reaction Steps
A solution of 1-methyl-1,3-dihydro-2H-benzimidazol-2-one (2 g, 13 mmoles) in DMF (50 ml) was added dropwise and at room temperature to a suspension of 80% sodium hydride (0.4 g, 13 mmoles) in DMF (25 ml). The mixture was heated at 40° C. for 30 minutes and cis-1,4-dichloro-2-butene (2.84 ml, 27 mmoles) in DMF (30 ml) was dropped in 4 hours under stirring. After stirring overnight at room temperature, the reaction mixture was poured into ice water and extracted with ethyl acetate. The organic layer was evaporated and the crude residue was purified by flash chromatography (hexane-ethyl acetate 55-45) to give 1.4 of the title compound as a thick yellowish oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06586435B2 |
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| Source dataset | uspto-grants-2003_07 |
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| ORD ID | ord-a9597ef213b948448daaebc9b2fb03e8 |
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| Source note | uspto-grants-2003_07 |
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