HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methoxyethanol → HCID 68209375, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methoxyethanol | HCID 8019 | — |
| Reactant | 2-Pyridyldiphenylphosphine | HCID 621893 | — |
| Reactant | Dibenzyl azodicarboxylate | HCID 5387121 | — |
| Reactant | 5-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one | HCID 136088927 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68209375 | HCID 68209375 | — |
Reaction Steps
40 mg (119 μmol) 5-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one, 19 μL (241 μmol) 2-methoxyethanol, 66 mg (251 μmol) diphenyl-2-pyridylphosphine and 10 ml THF are placed under protective gas. At 0° C. 58 mg (252 μmol) DBAD are added and then the mixture is stirred overnight at RT. Then it is diluted with EA and extracted with 10% sodium carbonate solution. The organic phase is stirred with 20 mL of 4N HCl for 5 min and then extracted. The organic phase is washed with saturated saline solution and then the solv. is eliminated i.V. The residue is purified on silica gel. (Eluant: DCM/MeOH/ammonia) The solv. of the corresponding fractions is eliminated i.V. and the residue is crystallised with cyclohexane/EA.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772323B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-db4ecefdbb264fd4a8e0a3cf19be5029 |
| Source note | uspto-grants-2014_07 |