Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1-Chloromethylnaphthalene | HCID 6845 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178518919 | HCID 178518919 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 2470061 | HCID 2470061 | 67.6% |
Reaction Steps
9.0 g (65 mmol) of potassium carbonate were added to a solution of 10.0 g (60.61 mmol) of 4,5-dichloro-3-hydroxy-pyridazine in 50 ml dimethylsulphoxide, then 9.42 g (63 mmol) of 1-(chloromethyl)-naphthalene were added and the mixture was stirred for 17 hours at 50° C. The dark solution was cooled and then combined with 300 ml of dist. water, then 300 ml dichloromethane were stirred in, the mixture was suction filtered through Celite, the aqueous phase was separated off and extracted another three times with 50 ml of dichloromethane. The combined organic phases were washed with water, dried over sodium sulphate and evaporated down. The crude product thus obtained was dissolved in 250 ml dichloromethane, the solution was filtered through silica gel and then evaporated down. The residue was triturated with petroleum ether, suction filtered and dried.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07109192B2 |
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| Source dataset | uspto-grants-2006_09 |
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| ORD ID | ord-ae52026fb9a54e67bd75373be3921540 |
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| Source note | uspto-grants-2006_09 |
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