HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 117643582, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Reactant | 3-Iodo-1-methyl-5-nitro-1H-indazole | HCID 56773842 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 117643582 | HCID 117643582 | 20.3% |
Reaction Steps
Pyrrolidine (90 mg), cesium carbonate (500 mg), Pd2(dba)3 (46 mg), and Xantphos (58 mg) were added to a dioxane solution (4 ml) containing 3-iodo-1-methyl-5-nitro-1H-indazole (303 mg) obtained in the 1st step, followed by microwave irradiation (Initiator™, 160° C., 15 minutes, 2.45 GHz, 0-240 W). Then, ethyl acetate was added to the obtained residue, insoluble matter was removed by filtration, and the solvent was distilled away under reduced pressure. 1-Methyl-5-nitro-3-(pyrrolidine-1-yl)-1H-indazole (50 mg) was thus obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051310B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-2531a25d10764633a8e693522e28bd8c |
| Source note | uspto-grants-2015_06 |