HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 131717317, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(2-Pyridyl)piperazine | HCID 94459 | — |
| Reactant | 2-(Pyridin-2-yl)piperazine | HCID 19386830 | — |
| Reactant | 2-(2-Chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one | HCID 19819759 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 131717317 | HCID 131717317 | 103.7% |
Reaction Steps
To 50 mL of toluene was added 5.0 g (0.0171 mol) of 2-(2-chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one, 5.58 g (0.034 mol) of 2-(2-pyridyl)piperazine, and 3.4 g (0.034 mol) of triethylamine, and the entire reaction mixture heated to reflux. After 2 days, 1.5 g (0.009 mol) of 1-(2-pyridinyl)piperazine was added and reflux continued for 24 hours. The reaction mixture was washed with 2×50 mL of 1N NaOH, dried over Na2SO4, filtered and concentrated by rotary evaporation. The residue was subjected to preparative HPLC using silica gel as the stationary phase and eluting with 5% triethylamine in acetone. Like fraction were combined affording ~4.0 g (55%) of a glass.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05109013 |
| Source dataset | uspto-grants-1992_04 |
| ORD ID | ord-26c75822307c4372a136825b8c3718b8 |
| Source note | uspto-grants-1992_04 |