Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Diphenylmethylidenehydrazine | HCID 79304 | — |
| Edukt | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Edukt | 7-fluoro-2-methyl-3H-benzimidazol-5-yl amine | HCID 68005307 | — |
| Lösungsmittel | 4-Methylmorpholine | HCID 7972 | — |
| Produkt | HCID 178432276 | HCID 178432276 | — |
Reaktionsschritte
In a separate reaction container, 7-fluoro-2-methyl-3H-benzimidazol-5-yl amine (100 mg, 0.44 mmol), lithium bis(trimethylsilyl) amide (190 mg, 1.1 mmol), and benzophenone hydrazone (94.3 mg, 0.48 mmol) were dissolved in N-methyl-morpholine (0.5 ml) under a nitrogen atmosphere. Then, the prepared solution containing the catalyst was added thereto. After deaeration, this was heated and stirred at 100° C. under a nitrogen atmosphere for two hours. The reaction mixture was cooled to room temperature, and then an aqueous solution of 6 M hydrochloric acid (0.5 ml) was added thereto. The organic layer was isolated, and concentrated under reduced pressure. Thus, crude N-benzhydrylidene-N′-(7-fluoro-2-methyl-1H-benzimidazol-5-yl)-hydrazine was obtained. The obtained crude product was used in subsequent reactions without being purified.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08829199B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-0522042ac78d4dc9b73fc28706cba004 |
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| Quellennotiz | uspto-grants-2014_09 |
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