HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 22271444, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 90093198 | HCID 90093198 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22271444 | HCID 22271444 | — |
Reaction Steps
To a solution of the methyl 5-[bis(tert-butoxycarbonyl)amino]-6-methoxynicotinate (1 g, 2.61 mmol) in THF (10 mL) at 0° C. was added LiOH.H2O (275 mg, 6.54 mmol) in water (2.5 mL) and the reaction allowed to stir at room temperature for 4 hours. The reaction was diluted with water (5 mL) and extracted into DCM twice (2×10 mL). The aqueous layer was acidified to pH=5 with 10% citric acid solution and extracted into DCM (4×20 mL). The organic layers were collected, washed with brine (10 mL), dried over sodium sulphate and concentrated in vacuo to afford the title compound that was used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09163021B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-9315d1ef3d8543ad99e22deee18dd9a5 |
| Source note | uspto-grants-2015_10 |