HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12582765, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 86733381 | HCID 86733381 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 12582765 | HCID 12582765 | — |
Reaction Steps
A mixture of 12.6 g of benzoyl chloride in 100 cc of ethylene chloride is added dropwise to a suspension of 25.6 g of 3-chloro-5,6,7,8-tetrahydropyrido [4,3-c]pyridazine maleate in 250 cc of ethylene chloride and 21.8 g of triethylamine within 18 minutes at room temperature while stirring. The mixture is stirred at room temperature for a further 14 hours, 200 cc of water are added, the organic phase is separated and concentrated to an oil in a vacuum. Upon adding ether/dimethoxyethane to this oil, crude 6-benzoyl-3-chloro-5,6,7,8-tetrahydropyrido[4,3-c]pyridazine is obtained. After recrystallization from absolute ethanol with the addition of a small amount of coal, the compound has a M.P. of 125°-127° (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03954754 |
| Source dataset | uspto-grants-1976_05 |
| ORD ID | ord-99cb6240385e464ba781f084351fa2f1 |
| Source note | uspto-grants-1976_05 |