Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ozone | HCID 24823 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 59532366 | HCID 59532366 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59532381 | HCID 59532381 | 35% |
Reaction Steps
A solution of (R)-6-allyl-3-((R)-1-(4-bromophenyl)ethyl)-6-(4-fluorophenyl)-1,3-oxazinan-2-one (334 mg, 0.80 mmol) in dry CH2Cl2 (20 mL) was treated with ozone at −78° C. until the reaction mixture became blue. Then the mixture was flushed with oxygen to remove excess ozone. To the above mixture was added NaBH4 (273 mg, 7 mmol) at 0° C. and the reaction mixture was stirred for 4 hrs at ambient temperature under nitrogen. The reaction mixture was washed with water and then extract with CH2Cl2 twice. The combined organic phases were dried over NaSO4, filtered and concentrated to give the residue, which was purified by preparative HPLC to afford (S)-3-((R)-1-(4-bromophenyl)ethyl)-6-(4-fluorophenyl)-6-(2-hydroxyethyl)-1,3-oxazinan-2-one (118 mg, 35%). 1H NMR (CD3OD): 1.50 (m, 3H), 2.12 (m, 2H), 2.29 (m, 2H), 2.50 (m, 1H), 3.10 (m, 1H), 3.33 (m, 1H), 3.68 (m, 1H), 4.56 (m, 1H), 5.50 (m, 1H), 6.86 (m, 2H), 7.10 (m, 2H), 7.30 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08575156B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-21d4bcbe50bf4a3d81412a38002f5218 |
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| Source note | uspto-grants-2013_11 |
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