HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-(2-Hex-5-ynoylperhydropyridazinyl)-3,3-dimethylpentane-1,2-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Isobutyl chloroformate | HCID 62365 | — |
| Edukt | 5-Hexynoic acid | HCID 143036 | — |
| Edukt | 3,3-Dimethyl-1-perhydropyridazinylpentane-1,2-dione | HCID 69417804 | — |
| Produkt | 1-(2-Hex-5-ynoylperhydropyridazinyl)-3,3-dimethylpentane-1,2-dione | HCID 18470065 | 63% |
Reaktionsschritte
To a solution of 5-hexynoic acid (0.467 g, 4 mmol) in 10 ml CH2Cl2was added triethylamine (0.56 ml, 4 mmol), followed by isobutyl chloroformate (0.53 ml, 4 mmol) at 0° C. After stirring for 5 minutes, a solution of 3,3-dimethyl-1-perhydropyridazinyl pentane-1,2-dione (0.424 g, 2 mmol) in 1 ml CH2Cl2was added. The reaction was gradually warmed up to room temperature. The crude material was subject to silica gel purification to yield final product as clear oil (0.385 g, 63%). 1H NMR (CDCl3, 400 MHz): δ 0.91 (t, 3H, J=7.0); 1.26 (s, 6H); 1.76(m, 8H); 2.28 (m, 2H); 2.50 (m, 2H); 2.88 (m, 2H); 3.60 (m, 1H); 4.50 (m, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07253169B2 |
| Quelldatensatz | uspto-grants-2007_08 |
| ORD ID | ord-31834923f74a48afa743f4d505a429d9 |
| Quellennotiz | uspto-grants-2007_08 |