HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 21246143, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4,5-Dichloro-3-hydroxypyridazine | HCID 73247 | — |
| Reactant | HCID 178418255 | HCID 178418255 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21246143 | HCID 21246143 | 73.4% |
Reaction Steps
Phenyl magnesium bromide (prepared from bromobenzene (171 g), magnesium (38.8 g) and diethyl ether (1.6 l)) was slowly added to a stirred solution of 4,5-dichloro-3[2H]-pyridazinone (60 g) in tetrahydrofuran (1 l) cooled at water bath temperature. This mixture was stirred at room temperature for 30 minutes and hydrolysed with 20% ammonium chloride solution (800 ml) in the cold. The aqueous layer was extracted with diethyl ether and the combined organic extracts were washed with dilute hydrochloric acid, water, brine, dried (MgSO4) and evaporated under reduced pressure to give 5-chloro-4-phenyl-3[2H]-pyridazinone (55.13 g), m.p. 193°-5° C. on recrystallisation from ethyl acetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04820819 |
| Source dataset | uspto-grants-1989_04 |
| ORD ID | ord-4b02b8b49a234dbdb1bd95cf3ef70c18 |
| Source note | uspto-grants-1989_04 |