HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22339441, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | HCID 22339372 | HCID 22339372 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22339441 | HCID 22339441 | — |
Reaction Steps
To a stirred solution of 2-(3-chloro-4-{3-[(4-fluoro-phenyl)-hydroxy-methyl]-4-hydroxy-phenoxy}-5-methyl-phenyl)-2H-[1,2,4]triazine-3,5-dione (0.4 g) in dichloromethane (25 mL) were added methanesulfonic acid (0.7 mL) and triethylsilane (1.5 mL) portionwise over 1 h. After a total of 1.5 h, water was added, the layers separated and the aqueous layer extracted with dichloromethane. The combined organic layers were washed with saturated sodium bicarbonate, dried (Na2SO4), concentrated in vacuo and flash chromatographed on silica gel (10-50% THF/hexanes) to afford the title compound of this EXAMPLE as a colorless foam, 56 mg. MS Calc.:453.9; Found:452.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06930107B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-e911db4c5a5b4e7999660835a39c3e65 |
| Source note | uspto-grants-2005_08 |