Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 131726954 | HCID 131726954 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131726953 | HCID 131726953 | 93.1% |
Reaction Steps
5.68 g (11 mmol) of the resulting alcohol derivative were dissolved in methylene chloride (60 ml) followed by the addition of 2.3 ml (16.5 mmol) of triethylamine under a nitrogen atmosphere, the addition of 1.02 ml (13.2 mmol) of methanesulfonyl chloride with ice-cooling, and stirring for 30 minutes at room temperature under a nitrogen atmosphere. Water was then added to the reaction solution followed by washing the methylene chloride layer with water and a saturated aqueous solution of sodium chloride and drying with anhydrous magnesium sulfate. After filtering, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=3/2) to obtain 6.09 g of the desired compound (93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07396930B2 |
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| Source dataset | uspto-grants-2008_07 |
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| ORD ID | ord-499d2b9beb5c423295c9da9febc7ca90 |
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| Source note | uspto-grants-2008_07 |
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