HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → 6-(((Tert-butoxy)carbonyl)(ethyl)amino)pyridine-3-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | 6-(Tert-butoxycarbonyl-ethyl-amino)-nicotinic acid methyl ester | HCID 66770142 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 6-(((Tert-butoxy)carbonyl)(ethyl)amino)pyridine-3-carboxylic acid | HCID 66769552 | — |
Reaction Steps
The crude 6-(tert-butoxycarbonyl-ethyl-amino)-nicotinic acid methyl ester is taken up in 100 mL dioxane and a solution of lithium hydroxide monohydrate (13.5 g, 0.32 mol) in 100 mL water is added and the reaction mixture is stirred at RT for 4 h. The dioxane is removed from the reaction mixture under reduced pressure, additional water is added and the reaction mixture is acidified to pH 6 with a solution of 10% citric acid in water. The formed precipitate is filtered off and dried in vacuo. Yield: 36 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09243000B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-ae37f5cd843040dd91b1de31adfa9b38 |
| Source note | uspto-grants-2016_01 |