Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Piperidine | HCID 8082 | — |
| Edukt | Tert-butyl 4-[(5-chloro-6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate | HCID 71278506 | — |
| Edukt | 5-chloro-1H-indazole-3-carbaldehyde | HCID 178520029 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178452318 | HCID 178452318 | 35,1% |
Reaktionsschritte
A solution of tert-butyl 4-[(5-chloro-6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate (0.100 g, 0.261 mmol) synthesized in Example B13, Step 2 in methanol (1 mL) was added with 5-chloro-1H-indazole-3-carbaldehyde (0.0471 g, 0.261 mmol) synthesized in Example B9, Step 3, and piperidine (0.00222 g, 0.0261 mmol) at room temperature, and the mixture was stirred at 60° C. for 1 hour. The reaction mixture was cooled to room temperature, then added with methanol (4 mL), and suspended in methanol and thereby washed to obtain tert-butyl (Z)-4-({5-chloro-2-[(5-chloro-1H-indazol-3-yl)methylene]-6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl}methyl)piperazine-1-carboxylate (0.050 g, 35%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09156827B2 |
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| Quelldatensatz | uspto-grants-2015_10 |
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| ORD ID | ord-2d144a4e202343e08ccedbd0e09a5f3a |
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| Quellennotiz | uspto-grants-2015_10 |
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