Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 22723091 | HCID 22723091 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | N,N-Dimethylethylenediamine | HCID 66053 | — |
| Product | HCID 12096929 | HCID 12096929 | — |
Reaction Steps
1,1′-Carbonyldiimidazole (0.43 g) was dissolved in a solution of 2-(dimethylamino) ethylamine (0.19 g) in anhydrous tetrahydrofuran (11 ml) in the nitrogen gas atmosphere and the resulting solution was stirred at room temperature for 20 minutes. To the reaction solution, there was added N-(2-hydroxyethyl)-2-cyclohexyl ethylamine hydrochloride (0.50 g) and the mixture was refluxed with heating for 3 hours. Chloroform was added to the reaction solution with ice cooling, followed by washing the mixture with saturated sodium hydrogen carbonate aqueous solution and then with saturated sodium chloride aqueous solution, drying over anhydrous magnesium sulfate and concentrating under reduced pressure. The resulting oily product was purified through the silica gel column chromatography to thus give the title compound (Compound 1-1, 0.68 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06683200B2 |
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| Source dataset | uspto-grants-2004_01 |
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| ORD ID | ord-f4bd15b6020d49cd9d1b603a73eceb94 |
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| Source note | uspto-grants-2004_01 |
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