Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178517393 | HCID 178517393 | — |
| Product | HCID 68074936 | HCID 68074936 | 59.5% |
Reaction Steps
To a solution of R109 (500 mg, 1.694 mmol) in pyridine (1.618 mL, 20 mmol) is added POCl3 (1.551 mL, 16.94 mmol) in a pressure flask. The reaction mixture is stirred at 90° C. for 18 hours. After this time, the reaction mixture is poured into ice water and extracted with EA twice. The organics are combined and washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude is purified by flash chromatography (SiO2, 5-40% EA/Heptane) to afford the title compound (316 mg); no ionization.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08580829B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-8f3b11b386e94a0e8216bd96019cd1a4 |
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| Source note | uspto-grants-2013_11 |
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