HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 59509102, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 59509124 | HCID 59509124 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59509102 | HCID 59509102 | — |
Reaction Steps
To a solution of 1-[6-(2-methoxy-phenyl)-pyrimidin-4-ylcarbamoyl]-pyrrolidine-2-carboxylic acid methyl ester (LX) (500 mg, 1.40 mmol) in a mixture of THF and water (1:1) was added a solution of LiOH (0.118 g, 2.80 mmol) in water at ice bath temperature over 10 min and then allowed to stir for two hours at room temperature. THF was evaporated and the aqueous solution was acidified with 2N HCl. This aqueous phase was then extracted with ethyl acetate (2×100 ml), the combined organic phases were washed with water and brine, dried over anhydrous sodium sulfate and concentrated in a vacuum rotavapor to afford 1-[6-(2-methoxy-phenyl)-pyrimidin-4-ylcarbamoyl]-pyrrolidine-2-carboxylic acid as a white solid. Yield: 210 mg, 43.8%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08716296B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-a3fd876da137489896eb87c2447030cb |
| Source note | uspto-grants-2014_05 |