Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Isocyanic acid, p-methoxybenzyl- | HCID 187910 | — |
| Edukt | HCID 59593344 | HCID 59593344 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 24953576 | HCID 24953576 | — |
Reaktionsschritte
3-(3,5-dimethyl-1H-pyrazol-4-ylmethyl)-pyrrolo[2,3-b]pyridine-1-carboxylic acid tert-butyl ester (514, 10 mg, 0.03 mmol) was dissolved in dichloromethane (0.5 mL). 1,8-Diazabicylo[5.4.0]unde-7-ene (6 mg, 0.04 mmol) was added. 1-Isocyanatomethyl-4-methoxy-benzene (545, 6.5 mg, 0.04 mmol) was added. The reaction was allowed to proceed at room temperature for 30 minutes. Acetic acid (0.2 mL) was added to the reaction. The solvents were removed under reduced pressure. The residue was dissolved in dimethyl sulfoxide (0.2 mL) and purified by reverse phase HPLC on a Phenomenex column (50 mm×10 mm ID), eluting with water with 0.1% trifluoroacetic acid and 20-100% acetonitrile with 0.1% trifluoroacetic acid over 16 minutes at a flow rate of 6 mL/minute to provide the desired compound P-0135. MS (ESI) [M+H+]+=390.3.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08722702B2 |
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| Quelldatensatz | uspto-grants-2014_05 |
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| ORD ID | ord-58eb315e9d0c49b1a399d98137485ca3 |
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| Quellennotiz | uspto-grants-2014_05 |
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