HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → HCID 86714423, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | HOAt | HCID 181649 | — |
| Edukt | 1H-Pyrazol-1-ylacetic acid | HCID 3717462 | — |
| Edukt | Methyl 3-amino-4-(pentan-3-ylamino)benzoate | HCID 61311526 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 86714423 | HCID 86714423 | 47,4% |
Reaktionsschritte
To a solution of 1.76 g of Pyrazol-1-yl-acetic acid in 20 ml of dry DMF 2.09 g of HOAT, 3.75 g of EDC and 6.9 ml of DIPEA were added at 0° C. After 30 min 3.3 g of 3-amino-4-(1-ethyl-propylamino)-benzoic acid methyl ester were added and the reaction was stirred at rt for 16 h. The reaction was then poured into water and extracted with ethyl acetate three times. The combined organic phases were washed with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and concentrated. The crude product was purified by precipitation from heptane to yield 2.28 g (47%) of 4-(1-Ethyl-propylamino)-3-(2-pyrazol-1-yl-acetylamino)-benzoic acid methyl ester.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09156796B2 |
| Quelldatensatz | uspto-grants-2015_10 |
| ORD ID | ord-46a0fd65e85b4c668f72f27a7ad43e38 |
| Quellennotiz | uspto-grants-2015_10 |