HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86668981, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 67120050 | HCID 67120050 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 86668981 | HCID 86668981 | 100% |
Reaction Steps
A solution of 5-(4,4-dimethoxy-2-methylbutanoyl)-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile (33 mg, 0.09 mmol) in CHCl3 (1.5 mL) was added TFA (0.4 mL) and water (0.4 mL) and the reaction was stirred 3 h at room temperature. The mixture was diluted with saturated aqueous solution of NaHCO3 and CH2Cl2. The organic phase was separated and the aqueous phase was extracted with CH2Cl2. The organic phase was then washed with saturated aqueous solution of NaHCO3. The combined extracts were dried with a phase separator and concentrated. The desired 1-(2-fluoro-4-methoxyphenyl)-3-methyl-5-(2-methyl-4-oxobutanoyl)-1H-pyrazole-4-carbonitrile (29 mg, 100%) was obtained and used immediately in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653112B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-e3936e58a5c94334ae31c7a46cdfe970 |
| Source note | uspto-grants-2014_02 |