HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Iodo-5-nitro-1-trityl-1H-indazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trityl chloride | HCID 6456 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178526495 | HCID 178526495 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-Iodo-5-nitro-1-trityl-1H-indazole | HCID 22260816 | 95.9% |
Reaction Steps
To a solution of 27.5 g of 3-iodo-5-nitro-1H-indazole in 300 ml tetrahydrofuran at 0° C. in an atmosphere of nitrogen gas was added 6.1 g of 60% sodium hydride, and the mixture was stirred at the same temperature for 10 minutes. To the mixture was added 39.8 g of trityl chloride, followed by stirring at room temperature for 1 hour. Water was added and the mixture was diluted with ethyl acetate. The organic layer was sequentially washed with saturated aqueous ammonium chloride solution and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated. The resulting crude crystals were washed with diethyl ether, to give 48.5 g of the title compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06982274B2 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-a9838a8399f34b5f8aa72dd636381270 |
| Source note | uspto-grants-2006_01 |