Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 86711613 | HCID 86711613 | — |
| Product | HCID 86711612 | HCID 86711612 | — |
Reaction Steps
To a solution of preparation 4a (1.8 g, 90% purity, 6.95 mmol) in methanol (5 mL) is added slowly thionyl chloride (1.64 g, 13.8 mmol) at 0° C. The reaction mixture is stirred at 70° C. for 1.5 h, concentrated under reduced pressure and purified by reversed-phase HPLC (Gilson: Sunfire, 30° C., gradient of acetonitrile in water+0.1% formic acid). Yield: 199 mg (12% of theory). ESI mass spectrum: [M+H]+=248; r.t. HPLC: 0.56 min (Z018_S04).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09346794B1 |
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| Source dataset | uspto-grants-2016_05 |
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| ORD ID | ord-7cf0e3abd5064bf2a84e3b80bffea3a0 |
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| Source note | uspto-grants-2016_05 |
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