Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | (Methoxycarbonylsulfamoyl)triethylammonium hydroxide | HCID 11032497 | — |
| Edukt | Tert-butyl 4-(4-carbamoyl-2-oxo-2,3-dihydroimidazol-1-yl)piperidine-1-carboxylate | HCID 59006367 | — |
| Lösungsmittel | 1,1-Dichloroethane | HCID 6365 | — |
| Produkt | HCID 59006363 | HCID 59006363 | 54,5% |
Reaktionsschritte
(Methoxycarbonylsulfamoyl)triethylammonium hydroxide, inner salt (179.7 mg, 0.754 mmol) was added to a solution of tert-butyl 4-[4-(aminocarbonyl)-2-oxo-2,3-dihydro-1H-imidazol-1-yl]piperidine-1-carboxylate (78 mg, 0.251 mmol) in dichloroethane (5 mL) and was heated to 50° C. After 1 h, the reaction was worked up with dichloromethane and saturated sodium bicarbonate. The organic extracts were washed with brine, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane→5% methanol {1% ammonium hydroxide}/dichloromethane) gave the title compound (40 mg). MS 237.04 (M+1-tert butyl)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07632832B2 |
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| Quelldatensatz | uspto-grants-2009_12 |
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| ORD ID | ord-05f908f0430b4cd795b481588415ca9f |
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| Quellennotiz | uspto-grants-2009_12 |
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