HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | (2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-carbamic acid tert-butyl ester | HCID 67773976 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | 2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine | HCID 67774145 | 95.9% |
Reaction Steps
A suspension of (2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-carbamic acid tert-butyl ester (8.5 g, 27.4 mmol) in hydrochloric acid (6 N in diethyl ether, 175 ml) is stirred overnight at room temperature. The suspension is diluted under cooling with water (ca 2 l) and ethyl acetate, the aqueous layer is washed once with ethyl acetate, made alkaline with 32% aqueous sodium hydroxide and extracted twice with ethyl acetate. The combined organic layers are dried with magnesium sulfate and the solvent is removed in vacuo affording 2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine (5.52 g, 95.9%) as a light pink solid. mp.: 212-213° C. MS: m/z=211.2 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349824B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-6ad8e7224305471dab0873492dc88cd7 |
| Source note | uspto-grants-2013_01 |