Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 21916126 | HCID 21916126 | — |
| Reactant | 3-(Cycloundecen-1-yl)-1,2-diazacycloundec-2-ene | HCID 53630274 | — |
| Reactant | HCID 178470341 | HCID 178470341 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 20780214 | HCID 20780214 | — |
Reaction Steps
To a solution of 2-bromo-5-methyl-3H-imidazole-4-carboxylic acid ethyl ester (1.00 g, 4.291 mmol) and 2-bromo-N-(2,4,6-trimethyl-phenyl)-acetamide (1.209 g, 4.720 mmol) in a mixture of toluene (16 mL) and acetone (8 mL) was added diazabicycloundecene (0.71 mL, 4.720 mmol). The resulting solution was stirred at room temperature for 24 h. Methanol (10 mL) was added to dissolve the precipitate formed, followed by the addition of silica gel (25 g). The solvent was removed under reduced pressure to dryness and the residue was applied to a silica gel-packed column. The isolation of the product was achieved by column chromatography (hexanes-ethyl acetate 4:1 to 1:2). Yield—0.736 g (42%). 1H NMR (DMSO d-6, 500 MHz) δ 9.52 (s, 1H), 6.86 (s, 2H), 5.15 (br s, 2H), 4.25 (q, J=7.1 Hz, 2H), 2.38 (s, 3H), 2.21 (s, 3H), 2.11 (s, 6H), 1.30 (t, J=7.1 Hz, 3H); LC/MS: tR=1.46 min., MS: [M+H]=408.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07125990B2 |
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| Source dataset | uspto-grants-2006_10 |
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| ORD ID | ord-27c1d9ee27914a88821fd0cb7c176d4a |
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| Source note | uspto-grants-2006_10 |
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