Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 68080203 | HCID 68080203 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 77230708 | HCID 77230708 | — |
Reaction Steps
MsCl (248 mg, 2.169 mmol) was added to a stirred, cooled 0° C. mixture of the title compound from Step D (370 mg, 1.808 mmol) in CH2Cl2 (10 mL), followed by addition of Et3N (274 mg, 2.71 mmol). The mixture was stirred at 0° C. for 30 min. TLC showed no starting material left. The mixture was quenched with water (5 mL) and the mixture was washed with more water (10 mL). The organic fraction were washed with brine (saturated, 10 mL), dried (Na2SO4), filtered and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel Biotage 40S, eluting with EtOAc/hexane (2/8) to give the title compound as a colorless solid. 1H NMR (CDCl3, 500 MHz) δ 5.40 (s, 2H), 3.20 (s, 3H), 2.61 (s, 3H), 2.59 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09221834B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-1848cc41273e4f8aaa674f5077843cef |
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| Source note | uspto-grants-2015_12 |
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