HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethylene Glycol → 1-(2-Bromo-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethylene Glycol | HCID 174 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 1-Carbethoxy-4-(2-bromo-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine hydrochloride | HCID 21481145 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-(2-Bromo-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine | HCID 21481142 | — |
Reaktionsschritte
47.2 g of 1-carbethoxy-4-(2-bromo- 10,11-dihydro-dibenzo-[b,f]thiepin-10-yl)-piperazine hydrochloride, 585 ml of ethylene glycol, 32.8 g of potassium hydroxide and 1.95 ml of water are heated to 160° C for 90 minutes. Then the mixture is poured on to water and extracted with chloroform. The organic solution is extracted with 2-N hydrochloric acid. The hydrochloric acid solution is made alkaline, extracted with chloroform, washed with water, dried over magnesium sulphate and concentrated under reduced pressure. There is obtained crystalline 1-(2-bromo- 10,11-dihydro-dibenzo[b,f]-thiepin-10-yl)-piperazine of melting point 112°-115° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04006145 |
| Quelldatensatz | uspto-grants-1977_02 |
| ORD ID | ord-944a1a7cca644a06ba95625767282490 |
| Quellennotiz | uspto-grants-1977_02 |