HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67120074, compound → HCID 67120050, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67120074 | HCID 67120074 | — |
| Reactant | HCID 86668980 | HCID 86668980 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 67120050 | HCID 67120050 | 48% |
Reaction Conditions
| Temperature | -40 °C |
|---|
Reaction Steps
To 1-(2-fluoro-4-methoxyphenyl)-5-iodo-3-methyl-1H-pyrazole-4-carbonitrile (66 mg, 0.18 mmol) in Et2O (1.5 mL) at −78° C. was added n-BuLi (2.5 M solution in hexane, 0.1 mL, 0.24 mmol). After stirring for 15 min, N,4,4-trimethoxy-N,2-dimethylbutanamide was added in Et2O (1.5 mL). The reaction was stirred at −78° C. for 15 hours while warming to −40° C. The reaction was quenched with water and extracted using a mixture of Et2O and DCM. Drying using a phase separator followed by concentration and purification using silica gel (heptane-EtOAc, 1:0 to 0:1) afforded 5-(4,4-dimethoxy-2-methylbutanoyl)-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile (33 mg, 48%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921402B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-c17a1629901140dea1108df576bd6c59 |
| Source note | uspto-grants-2014_12 |