HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethylenetriamine → N,N''-Di-Z-diethylenetriamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethylenetriamine | HCID 8111 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Cyanobenzyl formate | HCID 22902948 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | 1,1-Dichloroethane | HCID 6365 | — |
| Produkt | N,N''-Di-Z-diethylenetriamine | HCID 4367374 | — |
Reaktionsschritte
4.87 g (47.2 mmol) of 1,4,7-triazaheptane as well as 5 ml of triethylamine are dissolved in 100 ml of dichloroethane. The solution of 15.22 g (94.4 mmol) of cyanobenzyl formate in 200 ml of dichloromethane is instilled in this solution within 3 hours. It is allowed to stir for 2 more days at room temperature, then evaporated to dryness in a vacuum, taken up in diethyl ether and washed with sodium bicarbonate solution. The ether solution is dried on sodium sulfate and evaporated to dryness in a vacuum. The residue is crystallized from a little ethanol. The title compound crystallizes into white needles. Yield: 11.46 g (65.7% of theory) Melting point: 73°-75° C. Elementary analysis: Cld: C 64.67 H 6.78 N 11.31 Fnd: C 64.82 H 6.64 N 11.28
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05514810 |
| Quelldatensatz | uspto-grants-1996_05 |
| ORD ID | ord-6ac3c6418cea49e387abfe8f7bb26db8 |
| Quellennotiz | uspto-grants-1996_05 |