HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86245085, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | 2-Methyl-2H-pyrazol-3-ylamine | HCID 136927 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86245085 | HCID 86245085 | 50.9% |
Reaction Steps
To a solution of 1-methyl-1H-pyrazole-5-amine (1.00 g, 10.3 mmol) and pyridine (1.01 ml, 12.4 mmol) in tetrahydrofuran (34 ml) was added 2,2,2-trichloroethyl chloroformate (1.71 ml, 12.4 mmol) with ice-cooling and the mixture was stirred at room temperature for 1 hour. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain the desired product (1.43 g, 50.8%) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-de621059310f4c4296f4c869080c49f8 |
| Source note | uspto-grants-2010_12 |