HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 86706450, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | HCID 86706451 | HCID 86706451 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86706450 | HCID 86706450 | 20.4% |
Reaction Steps
To a solution of (R)-tert-butyl 3-((2-oxoethyl)(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)amino)piperidine-1-carboxylate (0.5 g, 0.97 mmol) in CH3CN (2 mL) at rt, was added an aq. solution of NaH2PO4 (3 mL, 0.21 g, 1.75 mmol), aq. NaO2Cl (2 mL, 0.16 g, 1.75 mmol) and 30% H2O2 (0.17 ml, 1.5 mmol) at 0° C. The reaction mixture was warmed to rt and stirred for overnight. The organic phase was concentrated in vacuo to afford a residue that was dissolved in EtOAc, filtered and dried over Na2SO4, concentrated in vacuo and purified by column chromatography (Silica gel, gradient MeOH: CH2Cl2) to afford the titled compound (0.105 g, 20.38%). LCMS [M+1]: 530.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273028B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-90b14104737e4dc6b2bc94328db9f90c |
| Source note | uspto-grants-2016_03 |