HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 12472016, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | HCID 12471994 | HCID 12471994 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 12472016 | HCID 12472016 | — |
Reaction Steps
5 g. of 10-chloro-3-(chloromethyl)-7-methyl-5H-s-triazolo[4,3-d] [1,4]benzodiazepin-6(7H)-one from part (a) is suspended in 50 ml. of 1,2-dimethoxyethane. N-methylpiperazine (5.4 g.) is added to the suspension and the mixture is heated under reflux for 5 hours. The solvent is stripped off, 3N aqueous sodium hydroxide is added to the residue and the mixture is extracted with several portions of chloroform. The combined chloroform extracts are dried over sodium sulfate and the solvent is removed under vacuum to leave a residue which is recrystallized from absolute ethanol to yield 4 g. of the title compound, melting point 228.5°-230.5°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04020064 |
| Source dataset | uspto-grants-1977_04 |
| ORD ID | ord-ebed3198accb495b9e84ec0ff5af79d6 |
| Source note | uspto-grants-1977_04 |