HuagongsheHuagongshe Chemistry Print Report · For research reference only
1H-Pyrrolo(2,3-b)pyridine → 1H-Indazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1H-Pyrrolo(2,3-b)pyridine | HCID 9222 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | 5-Nitro-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid | HCID 46942118 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1H-Indazole | HCID 9221 | 82% |
Reaction Steps
To the Rink resin (corresponding to fragment A9 of table I, 11 g, 0.85 mmol/g, 9.35 mmol) in anhydrous DMF (15 ml), 5-nitro-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid (2.9 g, 14.03 mmol), TBTU (4.5 g, 14.03 mmol) and DIPEA (3.62 g, 28.05 mmol) were added. The reaction mixture was shaken at room temperature for 20 hours and then the resin was isolated by filtration. The resin was washed sequentially with DMF (25 ml), DCM (25 ml), DMF (25 ml), DCM (25 ml), MeOH (25 ml), DCM (25 ml), MeOH (25 ml), DCM (25 ml), MeOH (25 ml), TBME (25 ml×2) and dried in vacuo to give the resin bound 7-azaindole (12.5 g). 0.01 g of the resin were cleaved (1 ml of 40% TFA/DCM) to give an off-white solid (0.0014 mg, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07888508B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-34848b586af14af188f38b189712f92e |
| Source note | uspto-grants-2011_02 |