HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 10200811, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Dithionite | HCID 24489 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 22661020 | HCID 22661020 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10200811 | HCID 10200811 | 90% |
Reaction Steps
To a solution of 1-(4-methoxy-phenyl)-5-(4-methylthio-phenyl)-3-trifluoromethyl-1H-1,2,4-triazole (30 g, 0.08 mol) in CH2Cl2 (320 ml) was added portionwise MCPBA (47.2 g, 0.16 mol). The reaction mixture was stirred at room temperature for 1.5 h, then cooled to 0-5° C. and a sodium hydrosulfite solution (500 ml) was carefully added to maintain the temperature below 18-20° C. The pH was adjusted to 8 by the addition of NaOH 30%. The mixture was extracted with dichoromethane, the organic phase was washed with saturated brine, dried over sodium sulfate and evaporated. Flash chromatography on silica gel (toluene/ethyl acetate: 8/2 as the eluent) and recrystallization from ethanol yielded a white solid (29.42 g, 90%) m.p. 156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06803380B1 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-c85048fce965412b9872adb7ffbcde2e |
| Source note | uspto-grants-2004_10 |