Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | 4-(2,2-Dimethoxyethyl)-1,3-dihydro-2H-benzimidazol-2-one | HCID 57834971 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57834974 | HCID 57834974 | 16.3% |
Reaction Steps
4-(2,2-Dimethoxy-ethyl)-1,3-dihydro-benzoimidazol-2-one (435 mg, 1.96 mmol) was dissolved along with benzyl bromide (335 mg, 1.96 mmol) in 10 mL of anhydrous DMF. Potassium tert-butoxide (1.0 M in THF, 2.2 mL, 2.2 mmol) was added. The reaction mixture was stirred at room temperature for 90 minutes and then partitioned between ether and water. The organic phase was washed with brine and dried over Na2SO4. After filtration and removal of solvent under reduced pressure, the crude material was chromatographed to afford 1-benzyl-4-(2,2-dimethoxy-ethyl)-1,3-dihydro-benzoimidazol-2-one (100 mg, 16%). 1H NMR (CDCl3) δ 3.00 (2H, d, J=5.0 Hz), 3.40 (6H, s), 4.55 (1H, t, J=5.0 Hz), 6.75 (d, 1H, J=7.5 Hz), 6.84-6.95 (m, 2H), 7.23-7.35 (m, 5H), 8.95 (br s, 1H). 13C(CDCl3) δ 36.9, 44.9, 54.4, 105.6, 107.5, 118.8, 121.7, 124.0, 127.9, 128.0, 129.1, 129.2, 130.8, 136.7.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07582760B2 |
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| Source dataset | uspto-grants-2009_09 |
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| ORD ID | ord-29c8078f49114470a543717008d5a639 |
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| Source note | uspto-grants-2009_09 |
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