HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 58142730, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Methylthio-4H-1,2,4-triazole | HCID 575378 | — |
| Reactant | ethyl (2Z)-2-chloro-2-[(2-fluorophenyl)methylhydrazinylidene]acetate | HCID 58142732 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58142730 | HCID 58142730 | — |
Reaction Steps
Ethyl(2Z)-chloro[(2-fluorobenzyl)hydrazono]acetate (807 mg, 3.12 mmol) from example 2A, 5-(methylthio)-1H-1,2,4-triazole (359 mg, 3.12 mmol) and triethylamine (316 mg, 3.12 mmol) are dissolved in dioxane (5 ml) and heated under reflux for 6 h. This is followed by dilution with water and extraction with ethyl acetate. The organic phase is dried over sodium sulfate, and the crude product is purified by chromatography on silica gel (eluent: dichloromethane/methanol 50:1). 124 mg (9.5% of theory) of the desired product are obtained with 69% purity.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08114400B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-ced263f4cd55478fb73a13234c96c764 |
| Source note | uspto-grants-2012_02 |