HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 6H-Pyrido(2,3-b)(1,4)benzodiazepin-6-one, 5,11-dihydro-11-((2,4-dimethyl-1-piperazinyl)acetyl)-, monohydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 11-(Chloroacetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-one | HCID 120053 | — |
| Reactant | 1,3-Dimethylpiperazine | HCID 13152035 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 6H-Pyrido(2,3-b)(1,4)benzodiazepin-6-one, 5,11-dihydro-11-((2,4-dimethyl-1-piperazinyl)acetyl)-, monohydrochloride | HCID 3053218 | 20% |
Reaction Steps
8.6 gm of 11-chloroacetyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiaze-pin-6-one, 3.1 gm of sodium carbonate and 4.5 gm of 1,3-dimethyl-piperazine were refluxed in 100 ml of absolute ethanol for 3.5 hours. After suction filtration the filtrate was evaporated to dryness. The residue was then purified on a silica gel column. The obtained base was dissolved in ethanol by addition of hydrochloric acid to form the hydrochloride. After recrystallization from ethanol: M.p.: 301°-303° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04213984 |
| Source dataset | uspto-grants-1980_07 |
| ORD ID | ord-19e6b642e3014411bf56f28fe56be7de |
| Source note | uspto-grants-1980_07 |