Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 17954502 | HCID 17954502 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59749462 | HCID 59749462 | 97.8% |
Reaction Steps
[3-(4-Bromo-3-fluoro-phenyl)-4,5-dihydro-isoxazol-5-yl]-methanol (30 g, 112.4 mmol) was added to anhydrous dichloromethane (300 ml) followed by addition of triethylamine (21.8 ml, 157.3 mmol). The solution was cooled to 0° C. followed by drop wise addition of methane sulfonyl chloride (10.4 ml, 134.8 mmol). The reaction was stirred for 2 hours at 0° C. and then aqueous sodium bicarbonate (100 ml) was added. After further extraction with dichloromethane (2×100 ml), the organic layers were combined, dried over sodium sulfate, and concentrated in vacuo to give the desired product (38.7 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07396847B2 |
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| Source dataset | uspto-grants-2008_07 |
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| ORD ID | ord-807eed1964034e9295d6d2d594c9f68f |
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| Source note | uspto-grants-2008_07 |
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