HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 44325576, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3,6-Dichloropyridazine | HCID 67331 | — |
| Reactant | 1-Pyrrolidineethanol | HCID 76288 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 44325576 | HCID 44325576 | — |
Reaction Steps
175 mg (4.01 mmol, 55%) NaH are added to a solution of 0.50 mL (4.04 mmol) N-(2-hydroxyethyl)pyrrolidine in 50 mL THF at 0° C. The reaction solution is stirred for 60 min and heated to RT. 500 mg (3.26 mmol) 3,6-dichloro-pyridazine are added. The solution is stirred for 5 h at RT. 50 mL water are added and the aqueous phase is extracted with 100 mL EtOAc. The organic phase is extracted once with saturated NaCl solution and dried over Na2SO4. The solvent is eliminated i.vac. and further purification is carried out by column chromatography on silica gel (gradient: EtOAc to EtOAc/MeOH/NH3 9:1:0.1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08618132B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-e8f94771b4f441709db0e9da4bed8860 |
| Source note | uspto-grants-2013_12 |