HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 118235802, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium peroxymonosulphate | HCID 10313463 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 118235535 | HCID 118235535 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 118235802 | HCID 118235802 | — |
Reaction Steps
A solution of Example 268 (4 g, 9.697 mmol) in MeOH (150 mL) and acetone (20 mL) at 0° C. was treated with Oxone® (potassium peroxymonosulfate; 11.92 g, 19.39 mmol) in water (100 mL). The resulting suspension was allowed to warm to r.t. and stirred for 18 h. The reaction mixture was treated with water and extracted with DCM (4×300 mL). The combined organic layers were concentrated in vacuo. A portion of the resulting crude yellow solid (4.4 g, 100%) was further purified by preparative HPLC to give the title compound (56 mg was obtained from 130 mg of crude material) as a white solid. HPLC-MS (pH 10): MH+ m/z 445.6 [M+H]+, RT 1.54 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09309243B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-125f61291e0940d4968022b96ce34c79 |
| Source note | uspto-grants-2016_04 |