HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 1,2-Dibenzoyl-5-[4,4-bis(4-fluorophenyl)butyl]-hexahydro-1H-1,2,5-triazepin
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1,1'-(4-Bromobutylidene)bis[4-fluorobenzene] | HCID 93763 | — |
| Reactant | 1,2-dibenzoyl-1H-1,2,5-triazepine | HCID 21277231 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1,2-Dibenzoyl-5-[4,4-bis(4-fluorophenyl)butyl]-hexahydro-1H-1,2,5-triazepin | HCID 14390913 | — |
Reaction Steps
A mixture of 4,4-bis(4-fluorophenyl)butyl bromide (2.08 g), 1,2-dibenzoyl-1H-1,2,5-triazepine (2.0 g), powdered anhydrous sodium carbonate (2.71 g) and N,N-dimethylformamide (20 ml, dried over 4A molecular sieves) was stirred at room temperature under a nitrogen atmosphere for three days. The mixture was filtered and the filtrate was evaporated under oil pump vacuum to an oil. The oil was chromatographed on a column of silica gel; elution with ethyl acetate-dichloromethane (2:3) giving a major product. The hydrochloride salt of the titled compound was formed in ether from this material; wt. 2.0 g (52%), mp=216°-218°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04801706 |
| Source dataset | uspto-grants-1989_01 |
| ORD ID | ord-364d0c76dbe5453f83ccb691db5a60c2 |
| Source note | uspto-grants-1989_01 |