Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | (R)-tert-butyl 2-((2-(2,6-difluoro-4-(methylcarbamoyl)phenyl)-5-methyl-1H-benzo[d]imidazol-1-yl)methyl)morpholine-4-carboxylate | HCID 67173392 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 67173930 | HCID 67173930 | — |
Reaktionsschritte
(R)-tert-butyl 2-((2-(2,6-difluoro-4-(methylcarbamoyl)phenyl)-5-methyl-1H-benzo[d]imidazol-1-yl)methyl)morpholine-4-carboxylate (770 mg, 1.54 mmol) was dissolved in DCM (10.0 mL). Afterward, TFA (2.00 mL) was added to the mixture at 0° C. The resulting mixture was stirred at room temperature for 1 hr and then concentrated under reduced pressure. The crude (S)-3,5-difluoro-N-methyl-4-(5-methyl-1-(morpholin-2-ylmethyl)-1H-benzo[d]imidazol-2-yl)benzamide trifluoroacetic acid salt product was used without further purification (790 mg) in the next step. It was analyzed on analytical HPLC MS using the high pH gradient method (mobile phase: 5-95% B; A: H2O with 10 mM NH4CO3 and 0.375% NH4OH v/v; B: CH3CN; 2.25 min run; X-Bridge C18; column size: 2.1×30 mm; particle size: 5 μm). MS m/z 401.3 [M+H]+ (ESI), Rt 1.37 min.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08530467B2 |
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| Quelldatensatz | uspto-grants-2013_09 |
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| ORD ID | ord-0ca3b92738254c9b985b4ed3fbde0798 |
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| Quellennotiz | uspto-grants-2013_09 |
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