Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | HCID 67020069 | HCID 67020069 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24993728 | HCID 24993728 | — |
Reaction Steps
To a solution of the product of Step C (22 mmol) in 10 mL of CH2Cl2 at −78° C. was added 300 μL of phosgene (20% in toluene). After stirring at −78° C. for 15 min and at 0° C. for 30 min, the reaction mixture was concentrated. Chromatography on a Biotage 40+S cartridge using 1:1 v/v EtOAc/hexanes as the eluant afforded the title compound: 1H NMR δ 1.27 (s, 9H), 1.48 (s, 3H), 1.56 (s, 3H), 1.86 (t, J=12.2, 1H), 2.27 (m, 1H), 5.50 (m, 1H), 5.87 (m, 1H), 6.99 (d, J=8.0, 2H), 7.17 (d, J=8.0, 2H), 7.39 (m, 1H), 7.58-7.72 (m, 3H), 9.87 (br. s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07999107B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-801d4443a73446c68fedfda4bb9018be |
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| Source note | uspto-grants-2011_08 |
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