Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Ethyl cyclopropanecarboximidate | HCID 14518434 | — |
| Edukt | HCID 178496998 | HCID 178496998 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 178496995 | HCID 178496995 | 35,6% |
Reaktionsschritte
Under N2 atmosphere to a cold solution of methyl 7-amino-2-[(2-chloro-6-fluorophenyl)amino]-6-hydroxy-1H-benzimidazole-5-carboxylate (0.400 g, 1.05 mmol) in DCM (25 mL), was added HCl salt of ethyl cyclopropanecarboximidate (Intermediate-57, 0.234 g, 1.57 mmol) at 0° C. The reaction mass was stirred at 0-5° C. for 1 h and at RT for 24 h. The obtained crude was purified by column chromatography on neutral alumina eluting with 1.0-2.0% MeOH:DCM to afford 0.150 g of the desired product. (DMSO-d6): δ 1.23 (m, 4H), 2.26 (m, 1H), 3.88 (s, 3H), 6.75 (s, 1H), 7.39 (m, 1H), 7.51 (m, 2H), 7.70 (s, 1H), 9.37 (s, 1H), 11.59 (s, 1H); MS [M+H]+: 401.21.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08519149B2 |
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| Quelldatensatz | uspto-grants-2013_08 |
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| ORD ID | ord-0711593ed8774ad1b791117f9be7dc6e |
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| Quellennotiz | uspto-grants-2013_08 |
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