HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl orthoformate → 6-iodo-3-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-3H-imidazo[4,5-b]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl orthoformate | HCID 31214 | — |
| Reactant | 5-iodo-N2-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)pyridine-2,3-diamine | HCID 118114038 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 6-iodo-3-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-3H-imidazo[4,5-b]pyridine | HCID 118114002 | 87% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a stirred suspension of 5-iodo-N2-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)pyridine-2,3-diamine (11.67 g, 23.70 mmol) in ethanol (175 mL) was added triethyl orthoformate (8.90 g, 60.05 mmol) and p-toluenesulfonic acid monohydrate (0.23 g, 1.19 mmol). As the mixture was warmed to reflux, the solids dissolved to provide a brown solution. After 30 min, the reaction mixture was cooled to 0° C., resulting in the formation of a precipitate. The solids were isolated by filtration, washed with a small amount of cold ethanol, and dried to provide 10.34 g (87%) of 6-iodo-3-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-3H-imidazo[4,5-b]pyridine as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174986B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-f38345a59a784fc19caa427ba6015136 |
| Source note | uspto-grants-2015_11 |