Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ozone | HCID 24823 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 58485258 | HCID 58485258 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 42642289 | HCID 42642289 | 42% |
Reaction Steps
A solution of (R)-4-allyl-1-((S)-3,3-dimethylbutan-2-yl)-4-(4-fluorophenyl)tetrahydropyrimidin-2(1H)-one (285 mg, 0.90 mmol) in CH2Cl2 (5 mL) was treated with O3 till the mixture was turned blue. Then NaBH4 was added and the mixture was stirred at rt till the reaction was over. The reaction was quenched with H2O, and the mixture was extracted with EtOAc. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated to give the crude product, which was purified by preparative TLC to afford (S)-1-((S)-3,3-dimethylbutan-2-yl)-4-(4-fluorophenyl)-4-(2-hydroxyethyl)tetrahydropyrimidin-2(1H)-one (120 mg, 42%). LC-MS Method 1 tR=1.021, min, m/z=323.1; 1H NMR (CDCl3): 0.72 (s, 9H), 0.99 (d, 3H), 1.35-1.98 (m, 2H), 2.03-2.14 (m, 3H), 2.51 (m, 1H), 3.04 (m, 1H), 3.31 (m, 1H), 3.64 (m, 1H), 4.47 (m, 1H), 6.66 (s, 1H), 6.96-7.01 (m, 2H), 7.24-7.28 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08748444B2 |
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| Source dataset | uspto-grants-2014_06 |
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| ORD ID | ord-a046225324904d0486c810ad810fd7cd |
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| Source note | uspto-grants-2014_06 |
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