HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-Benzyl-7-benzylamino-3-bromo-2-methylpyrrolo[2,3-d]pyridazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 1-Benzyl-3-bromo-7-chloro-2-methylpyrrolo[2,3-d]pyridazine | HCID 19437770 | — |
| Solvent | Benzylamine | HCID 7504 | — |
| Product | 1-Benzyl-7-benzylamino-3-bromo-2-methylpyrrolo[2,3-d]pyridazine | HCID 19437753 | — |
Reaction Steps
A solution of 1.0 g (2.97 retool) of 1-benzyl-3 -bromo-7-chloro-2-methylpyrrolo [2,3-d]pyridazine in 5 ml of benzylamine is heated to 150° C. for 5 h and subsequently cooled to room temperature. The solution is then treated with 50 ml of water, adjusted to pH 6 with 2 N hydrochloric acid and extracted with 2×50 ml of dichloromethane. The organic extracts are dried over magnesium sulfate and concentrated. The residue which remains is chromatographed on silica gel (eluent: toluene/dioxane=2:1). After concentration of the fractions of Rf=0.25 and crystallization from diisopropyl ether, 1.01 g (84%) of the title compound are isolated. M.p.: 185°-188° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05534515 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-2e5701863f444b899a50f5f4626ae5ea |
| Source note | uspto-grants-1996_07 |