HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 68687439, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68685046 | HCID 68685046 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68687439 | HCID 68687439 | 37.5% |
Reaction Steps
(3R,4R) and (3S,4S)-4-Amino-1-[2-(3,4-dimethoxy-phenyl)-ethyl]-piperidine-3-carboxylic acid ethyl ester (262 mg) and lithium hydroxide (166 mg) in 5 ml THF, 5 ml MeOH and 1 ml H2O were stirred for 24 h at ambient temperature. The mixture was diluted with buffer pH 7 and extracted with AcOEt. The combined organic layers were washed with brine and dried over sodium sulfate. Removal of the solvent under reduced pressure gave an oil which was purified by column chromatography (Isolute SPE Flash NH2, AcOEt) and precipitated (AcOEt/heptane) to give 90 mg (37%) of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07683079B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-265f5af2f3d045878a3f2d94069dbff7 |
| Source note | uspto-grants-2010_03 |