Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 23394352 | HCID 23394352 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59588983 | HCID 59588983 | — |
Reaction Steps
To a stirring solution of (E)-tert-butyl-N-(3-fluoro-4-hydroxybut-2-enyl)carbamate (1.65 g, 8 mmol) in CH2Cl2 (30 mL) at 0° C. under nitrogen was added triethylamine (1.67 mL, 12 mmol) followed by methanesulfonyl chloride (0.74 mL, 9.6 mmol). The reaction was left to stir at 0° C. for 1 hr. All volatiles were removed under reduced pressure and the crude yellow residue was taken up in acetone (30 mL). The insoluble white precipitate (triethylammonium chloride) was filtered off and washed with acetone (10 mL). The filtrate containing the crude mesylate was used immediately for Procedure E.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08426587B2 |
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| Source dataset | uspto-grants-2013_04 |
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| ORD ID | ord-349ef3ae0eb04c5b964bf341a7b694f8 |
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| Source note | uspto-grants-2013_04 |
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