HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → (2S)-4-methyl-2-({(1S)-2,2,2-trifluoro-1-[4'-(methylsulfonyl)-1,1'-biphenyl-4-yl]ethyl}amino)pentan-1-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | (2S)-4-methyl-2-({(1S)-2,2,2-trifluoro-1-[4'-(methylthio)-1,1'-biphenyl-4-yl]ethyl}amino)pentan-1-ol | HCID 11502160 | — |
| Catalyst | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | (2S)-4-methyl-2-({(1S)-2,2,2-trifluoro-1-[4'-(methylsulfonyl)-1,1'-biphenyl-4-yl]ethyl}amino)pentan-1-ol | HCID 11647629 | — |
Reaction Steps
To a 0° C. solution of the sulfide (19 g) from Step 4 in toluene (400 mL) was added Na2WO4.2H2O (0.16 g) and Bu4NHSO4 (0.81 g). Then 30% hydrogen peroxide (12.2 mL) was slowly added and the mixture was stirred at room temperature for 4.5 hours. The mixture was poured slowly on a mixture of ice, dilute aqueous sodium thiosulfate and ethyl acetate. The organic layer was separated and the aqueous further extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with brine, dried with magnesium sulfate and the solvent were removed in vacuo to yield a residue which was purified on SiO2 using ethyl acetate and hexanes (1:1) as eluant to yield the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318748B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-46a2a10d8d9344aeb626bf05b2760529 |
| Source note | uspto-grants-2012_11 |