HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Propanol → 1H-Pyrrolo[2,3-b]pyridine-3-carboxylic acid, 1-(1,1-dimethylethyl)-5-nitro-, propyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Propanol | HCID 1031 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 1H-Pyrrolo[2,3-b]pyridine-3-carbonitrile, 1-(1,1-dimethylethyl)-5-nitro- | HCID 66924520 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | 1H-Pyrrolo[2,3-b]pyridine-3-carboxylic acid, 1-(1,1-dimethylethyl)-5-nitro-, propyl ester | HCID 66924518 | 88% |
Reaction Steps
To a suspension of 5.0 g (20.47 mmol) of 1-tert-butyl-5-nitro-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile in 125 mL of n-propanol, 7.78 g of p-toluensulfonic acid were added under stirring. The mixture was heated at reflux for 40 hours and then it was cooled to room temperature and diluted with 70 mL of tert-butyl methyl ether. The precipitate was filtered off and the clear filtrate was concentrated under vacuum to a small volume (about 40-50 mL). The suspension was cooled to −5/0° C. and kept at this temperature for 2 hours. The solid was filtered, washed with 20 mL of 1:1 mixture of n-propanol and tert-butyl methyl ether and dried to afford 5.50 g of the title compound as a cream-colored solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08198298B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-668c62337f25451aae9f96859c6d4982 |
| Source note | uspto-grants-2012_06 |