HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 86587230, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Potassium bisulfate | HCID 516920 | — |
| Reactant | HCID 86587231 | HCID 86587231 | — |
| Reactant | HCID 123643341 | HCID 123643341 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86587230 | HCID 86587230 | 75.1% |
Reaction Steps
The mixture of N-[(R)-1-{3-(1-tert-butoxycarbonyl-4-piperidyl)propionyl}-3-piperidylcarbonyl]-2(S)-(4-methoxycarbonylbenzoyl)amino-β-alanine (55 mg, 0.106 mmol) in water (0.5 mL), monosilylacetamide (1.0 g) and N-methylmorpholine (61 mL, 0.55 mmol) was added 1N LiOH solution (0.37 mL) at 5° C. After stirring for 40 minutes, the mixture was neutralized with 20% aqueous KHSO4 solution, then purified by an ODS column chromatography using Daisogel-120sp (10% CH3CN/water) and freeze-dried to give N-[(R)-1-{3-(4-piperidyl)propionyl}-3-piperidylcarbonyl]-2(S)-(4-carboxybenzoyl)amino-β-alanine (40 mg, 75.1%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06812235B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-54207647921c4dc39b32984a73228afc |
| Source note | uspto-grants-2004_11 |