HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → N-[4-[(Dibenz[b,f] [1,4]thiazepin-10(11H)-yl)carbonyl]phenyl]-2,4-dichlorobenzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| Edukt | 10,11-Dihydro-10-(4-aminobenzoyl)dibenz[b,f][1,4]thiazepine | HCID 54230002 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-[4-[(Dibenz[b,f] [1,4]thiazepin-10(11H)-yl)carbonyl]phenyl]-2,4-dichlorobenzamide | HCID 67625596 | 78,9% |
Reaktionsschritte
To a solution of 452 mg of 2,4-dichlorobenzoyl chloride in 6 ml of methylene chloride is added 0.6 g of 10-(4-aminobenzoyl)-10,11-dihydrodibenz[b,f] [1,4]thiazepine followed by 0.375 ml of triethylamine. The reaction mixture is stirred at room temperature for 18 hours. The reaction mixture is washed with 20 ml of water, 1N HCl, 1N Na2CO3, water and dried over MgSO4. The filtrate is evaporated in vacuo to give 0.72 g of yellowish solid which is purified by silica gel chromatography on thick layer plates by elution with 1:1 ethyl acetate-hexane to give 0.254 g of the desired product as ivory crystals, m.p. 112°-115° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05760031 |
| Quelldatensatz | uspto-grants-1998_06 |
| ORD ID | ord-d19f3f9439fd4e129494d2041d626a22 |
| Quellennotiz | uspto-grants-1998_06 |