HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trifluoroethanol → HCID 68108403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Methyl 3-amino-5-chloropyrazine-2-carboxylate | HCID 53417426 | — |
| Product | HCID 68108403 | HCID 68108403 | — |
Reaction Steps
A mixture of 2,2,2-trifluoro-ethanol (6.9 ml, 96 mmol) and cesium carbonate (1.56 g, 4.8 mmol) was stirred for 20 min, 3-amino-5-chloro-pyrazine-2-carboxylic acid methyl ester [28643-16-5] (600 mg, 3.2 mmol) was added and the mixture was stirred at rt for 42 h. To complete the reaction the mixture was heated to reflux for another 3 h. Saturated aq. NH4Cl was added and the mixture was extracted with EtOAc, the combined organic layers were washed with saturated aq. sodium chloride, dried with Na2SO4 and evaporated. The residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 3:7) to provide the title compound as colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09163011B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-7100da3fa84e4b8b99a86e3a5a4a9be3 |
| Source note | uspto-grants-2015_10 |