HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → 11-(2-(2-((Diethylamino)methyl)-1-piperidinyl)acetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 11-(Chloroacetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-one | HCID 120053 | — |
| Edukt | N,N-Diethyl-2-piperidinemethanamine | HCID 254287 | — |
| Lösungsmittel | 1-Propanol | HCID 1031 | — |
| Produkt | 11-(2-(2-((Diethylamino)methyl)-1-piperidinyl)acetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-one | HCID 107867 | 83,6% |
Reaktionsschritte
A mixture of 11-(chloroacetyl)-5,11-dihydro-6H-pyrido-[2,3-b][1,4]benzodiazepin-6-one (97.6 g, 0.339 mol), 2-[(diethylamino)methyl]piperidine (64.0 g, 0.376 mol), sodium carbonate (36.0 g, 0.34 mol) and n-propanol (1.7 liters) is refluxed for 5 hours. The reaction mixture is filtered while hot then left to stand for 12 hours at ambient temperature, after which the desired product is found to have precipitated in crystalline form. The substance is suction filtered, washed 3 times, each time with n-propanol (100 ml), and dried in a vacuum drying chamber. Colorless crystals (119.5 g) are obtained, Mp. 226°-229° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04550107 |
| Quelldatensatz | uspto-grants-1985_10 |
| ORD ID | ord-a8b470b2578843f7be5ae99f60b3f865 |
| Quellennotiz | uspto-grants-1985_10 |