Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 54516649 | HCID 54516649 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57899277 | HCID 57899277 | — |
| Product | HCID 57899299 | HCID 57899299 | — |
Reaction Steps
A mixture of 4-(2-hydroxy-ethyl)-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-one (700 mg, 3.01 mmol), triethylamine (0.84 mL, 6.0 mmol), and methyl sulfonyl chloride (0.28 mL, 3.6 mmol) in dichloromethane (5.0 mL) was stirred at room temperature for 4 h. The reaction mixture was treated with saturated ammonium chloride and extracted with ethyl acetate. The combined organics were dried over Na2SO4, filtered and concentrated in vacuo. Purification via silica gel column chromatography provided methanesulfonic acid 2-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-ethyl ester (384 mg) and 4-(2-chloro-ethyl)-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-one (310 mg) in 41% combined yield. LCMS 311.3 (M+1) and LCMS 251.3 (M+1), respectively.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07943652B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-7bdb435f93154e469cd4e059b00a6a9e |
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| Source note | uspto-grants-2011_05 |
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