Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Methyl 4-fluoro-5-methanesulfonyl-2-methylbenzoate | HCID 10538364 | — |
| Reactant | 3,3-Difluorocyclobutanol | HCID 22500954 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 22500955 | HCID 22500955 | 75.6% |
Reaction Steps
370 mg of methyl 4-fluoro-5-methanesulfonyl-2-methylbenzoate, 297 mg of 3,3-difluorocyclobutanol and 1.47 g of Cs2CO3 were dissolved in 10 ml of anhydrous NMP and stirred at 60° C. for 4 h. The reaction mixture was then diluted with 125 ml of a 50% concentrated aqueous NaHCO3 solution and extracted 3 times with 100 ml of EA each time. It was dried over Na2SO4, and the solvent was removed in vacuo. Chromatography on silica gel with DIP resulted in 380 mg of a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06878748B2 |
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| Source dataset | uspto-grants-2005_04 |
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| ORD ID | ord-f50d7cbb377e49ed9ab00b73cc6c2f55 |
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| Source note | uspto-grants-2005_04 |
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