HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Isopropyl chloroformate → HCID 178459833, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Isopropyl chloroformate | HCID 7917 | — |
| Edukt | 3-Carboxybenzaldehyde | HCID 12077 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 5-Nitropyridine-2,3-diamine | HCID 3480151 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | HCID 178459833 | HCID 178459833 | — |
Reaktionsschritte
was prepared starting from 3-carboxybenzaldehyde and 2,3-diamino-5-nitropyridine as described for 10-1. In the final step, after reacting with isopropyl chloroformate in NMP, the reaction mixture was treated with 100 mg sodium hydroxide and 1 ml water for 1 hr at room temperature. The crude product was precipitated by addition of 30 ml water and filtered off. It was further purified by dissolving in 50 ml aqueous sodium carbonate solution and washing with dichloromethane. The carbonate solution was acidified to pH 2-3 by addition acetic acid and HCl, and extracted with dichloromethane. The dichloromethane phase was evaporated to give 61 mg of the title product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07786113B2 |
| Quelldatensatz | uspto-grants-2010_08 |
| ORD ID | ord-abbb1f9db501497e9bd603e6d6612106 |
| Quellennotiz | uspto-grants-2010_08 |