HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium → HCID 68805556, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium | HCID 5462222 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | HCID 68804660 | HCID 68804660 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68805556 | HCID 68805556 | — |
Reaction Steps
To a solution of 5-fluoro-6-(2-fluoro-4-iodo-phenylamino)-3-methyl-3H-benzoimidazole-5-carboxylic acid methyl ester (136.3 g, 0.305 mol) in tetrahydrofuran (1.5 L) was added potassium trimethylsilonate (155.95 g, 1.23 mol) at room temperature (after completion of the addition the reaction mixture became dark brown solution). The reaction mixture was stirred for 3.5 h (completion of reaction is confirmed by TLC-DCM:MeOH 1:9), quenched with water (25 ml) and evaporated under vacuum to remove THF. The residue was then adjusted to pH 1 with conc. HCl and the solid (creamy white) was filtered, washed with water (2×200 ml) then dried to give title compound. Yield: 96 g (52.53%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07160915B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-356a43a108cd43409e238b0389642594 |
| Source note | uspto-grants-2007_01 |