HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 5-Nitro-2-(2-(pyrrolidin-1-yl)ethyl)-2H-indazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Nitroindazole | HCID 21501 | — |
| Reactant | 1-(2-Chloroethyl)pyrrolidine hydrochloride | HCID 81668 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 5-Nitro-2-(2-(pyrrolidin-1-yl)ethyl)-2H-indazole | HCID 22138904 | — |
Reaction Steps
10.5 g (62.0 mmol) 1-(2-chloroethyl)-pyrrolidine hydrochloride and 12.9 g (93.0 mmol) K2CO3 are added successively to a solution of 5.00 g (31.0 mmol) 5-nitroindazole in 100 mL acetonitrile. The reaction solution is stirred for 2 h at RT and refluxed for a further 5 h. After the solution has cooled the insoluble salts are filtered off and the solvent is eliminated i.vac. The residue is taken up in EtOAc and water. The organic phase is dried over MgSO4 and the solvent is eliminated i.vac. A 4:1 mixture of 5-nitro-1-(2-pyrrolidin-1-yl-ethyl)-1H-indazole and 5-nitro-2-(2-pyrrolidin-1-yl-ethyl)-2H-indazole is obtained. The purification is carried out by column chromatography on Alox (PE/EtOAc 3:2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08618132B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-36d3bb82adf84e00976ec3ad6c4152da |
| Source note | uspto-grants-2013_12 |