Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Oxalyl chloride | HCID 65578 | — |
| Edukt | 2-Amino-4-fluorobenzamide | HCID 10241004 | — |
| Edukt | Bromo(4-fluorophenyl)acetic acid | HCID 16217752 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 66610889 | HCID 66610889 | — |
Reaktionsschritte
To a solution of 2-bromo-2-(4-fluorophenyl)acetic acid (425 mg, 1.82 mmol) in DCM (5 mL) and DMF (0.05 mL) was added oxalyl chloride (0.17 mL, 1.91 mmol) and the solution was stirred for 0.75 h. The solution was then cooled to 0° C. and a solution of 2-amino-4-fluorobenzamide (267 mg, 1.73 mmol) in pyridine (1 mL) was added. The solution was stirred at rt for 1 h and then evaporated. The crude residue was partitioned between EtOAc and 2 N HCl. The EtOAc layer was evaporated to give 2-(2-bromo-2-(4-fluorophenyl)acetamido)-4-fluorobenzamide as a crude oil which was used without further purification. (420 mg, 62%). LC-MS (ESI) m/z 369 (M−H)—.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09308207B2 |
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| Quelldatensatz | uspto-grants-2016_04 |
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| ORD ID | ord-6d6a742a0aa540a0a63b152078c2fb70 |
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| Quellennotiz | uspto-grants-2016_04 |
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