Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | HCID 57743007 | HCID 57743007 | — |
| Reactant | HCID 178418918 | HCID 178418918 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57742996 | HCID 57742996 | 83.2% |
Reaction Steps
In a reaction vessel under inert atmosphere, 4-iodo-3,5-dimethyl-1-[(4-methylphenyl)sulfonyl]-1H-pyrazole x53 (1.44 g, 3.8 mmol) is dissolved in dry THF (10 ml) and cooled down to −73° C. A 2M solution of isopropylmagnesiumchloride in THF (9.6 mmol, 4.8 ml) is added dropwise and the mixture is stirred at −73° C. for 1 h. Then 0.44 ml of DMF (5.7 mmol) are added and the solution stirred at room temperature overnight. DMF (1.9 mmol) is further added and stirring is continued for 16 h. The reaction mixture is quenched with a saturated solution of NH4Cl, extracted three times with CH2Cl2, the organic phase is washed with brine, dried over MgSO4, filtered and concentrated in vacuo to give 0.88 g of crude 3,5-dimethyl-1-[(4-methylphenyl)sulfonyl]-1H-pyrazole-4-carbaldehyde x56, which is used in the next step without any further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08178533B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-fe3191dd8fea43dfa74518e3442783c4 |
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| Source note | uspto-grants-2012_05 |
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