HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-dihydro-2H-pyran → 4-Bromo-5-methyl-1-(tetrahydro-pyran-2-yl)-3-trifluoromethyl-1H-pyrazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | 4-Bromo-3-methyl-5-(trifluoromethyl)pyrazole | HCID 2736430 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-Bromo-5-methyl-1-(tetrahydro-pyran-2-yl)-3-trifluoromethyl-1H-pyrazole | HCID 59331983 | 72.1% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of 4-bromo-5-methyl-3-trifluoromethyl-1H-pyrazole (1.4 g, 6.2 mmol, 1.0 equiv) in chloroform (31 ml) was added p-toluene sulphonic acid monohydrate (118 mg, 0.62 mmol, 0.1 equiv). The solution was cooled to 0° C. and 3,4-dihydro-2H-pyran (0.85 ml, 9.3 mmol, 1.5 equiv) was added drop-wise over 5 minutes. The mixture was allowed to warm to room temperature for 1 hour and the solvents were removed under reduced pressure. The crude mixture was purified by column chromatography (SiO2), eluting with 0→25% EtOAc-petrol over a linear gradient to afford the title compound 1.4 g (59%), LCMS (PS-A) Rt 3.72 min [M+H]+ 314.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247576B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-af5c0cca244742ddbf219a4ca7fe7770 |
| Source note | uspto-grants-2012_08 |