HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → 5-Methyl-6-(piperidine-1-sulfonyl)-pyridine-2-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | 5-Methyl-6-(piperidine-1-sulfonyl)-pyridine-2-carboxylic acid methyl ester | HCID 71087882 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 5-Methyl-6-(piperidine-1-sulfonyl)-pyridine-2-carboxylic acid | HCID 71087855 | 71.1% |
Reaction Steps
5-Methyl-6-(piperidine-1-sulfonyl)-pyridine-2-carboxylic acid methyl ester (53 mg, 0.178 mmol) in dioxane (2 mL) was added to a solution of lithium hydroxide monohydrate (CAN 1310-66-3, 0.1 g, 2.38 mmol) in water (2 mL) and the mixture was stirred for 2 h at room temperature. The solvent was removed in vacuo, water (10 mL) was added, and the pH was adjusted to 3 with 1 N hydrochloric acid. The mixture was extracted by ethyl acetate (2×10 mL). The organic layer was washed with brine (20 mL), dried over anhydrous sodium sulfate, and concentrated to give the product (36 mg, 71%); MS (EI): m/e=285.2 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09321727B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-19de1a4da335470f8a0980ceee6fa690 |
| Source note | uspto-grants-2016_04 |