HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiourea → HCID 178527723, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | 3-(Benzyloxy)-6-chloropyridazine | HCID 22506957 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 178527723 | HCID 178527723 | 15.2% |
Reaction Steps
A mixture of 3-benzyloxy-6-chloro-pyridazine (18.2 mmol, 4 g), thiourea (36.3 mmol, 2.8 g) and ethyl methyl ketone (75 mL) was refluxed overnight. Excess ethyl methyl ketone was evaporated, the residue was extracted with 2M sodium hydroxide (25 mL) and the sodium hydroxide solution was washed with EtOAc (2×30 mL). The aqueous layer was collected and sufficient conc. HCl was added to bring the pH to 5 and extracted with EtOAc (2×30 mL). The EtOAc extract was collected, dried, filtered and the filtrate was evaporated to yield 3-benzyloxy-6-mercapto-pyridazine (15%, 605 mg); mp 155° C.-157° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06849629B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-df9c3c46233e4d73b1173ac3874fed00 |
| Source note | uspto-grants-2005_02 |