Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Phenethylamine | HCID 1001 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3-Fluorobenzoyl chloride | HCID 74376 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 3-fluoro-N-(2-phenylethyl)benzamide | HCID 762737 | 85.617,797% |
Reaktionsschritte
174.9 ml (1.39 mol) of phenylethylamine were dissolved in 600 ml of dichloromethane and admixed with 196.0 ml (1.41 mol, 1.01 eq.) of triethylamine. Subsequently, 221.0 g (1.39 mmol) of 3-fluorobenzoyl chloride were added dropwise to the solution at 0° C. such that the temperature did not rise above 40° C. The mixture was stirred at RT for 18 h and the precipitated solid was dissolved in 1000 ml of dichloromethane. The mixture was washed four times with 200 ml of dilute NaOH, 1N HCl and saturated NaHCO3 solution. The organic phase was removed, dried over MgSO4 and concentrated under reduced pressure. The solid was filtered off with suction and washed twice with a little dichloromethane. 289.52 g of a white solid were obtained with >99% purity (by HPLC), corresponding to 85.4% of theory.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07820822B2 |
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| Quelldatensatz | uspto-grants-2010_10 |
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| ORD ID | ord-19b5d28b536a414b98ba7c271657e4fc |
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| Quellennotiz | uspto-grants-2010_10 |
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