HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-Methylbutylamine → Methyl 3-{[butyl(methyl)amino]carbonyl)-5-iodobenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-Methylbutylamine | HCID 8068 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Edukt | 3-Iodo-5-(methoxycarbonyl)benzoic acid | HCID 15840391 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Methyl 3-{[butyl(methyl)amino]carbonyl)-5-iodobenzoate | HCID 21086165 | — |
Reaktionsschritte
3-Iodo-5-(methoxycarbonyl)benzoic acid (1 g, 3.3 mmol) is dissolved in DMF (10 mL), and diisopropylethylamine (1.7 mL, 9.8 mmol), HATU (1.5 g, 3.9 mmol), and N-methylbutylamine (581 μL, 4.9 mmol) are added. The reaction stirred at room temperature 2 h. The reaction is partitioned between ethyl acetate and water. The organic layer is washed with saturated sodium bicarbonate, and saturated sodium chloride, dried (sodium sulfate), filtered, and concentrated under reduced pressure. Purification by flash column chromatography (silica, 40% ethyl acetate/hexane) provides the title compound. ESI MS m/z 376.1 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07176242B2 |
| Quelldatensatz | uspto-grants-2007_02 |
| ORD ID | ord-8a500f39426944db86cb3eecd30559c4 |
| Quellennotiz | uspto-grants-2007_02 |