HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12986046, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 69679879 | HCID 69679879 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12986046 | HCID 12986046 | 99.7% |
Reaction Steps
Lithium aluminum hydride (6.0 g, 0.16 mmol) is suspended in THF (500 ml), and thereto is added with stirring 3-(3-methoxymethoxypyridin-4-yl)propionic acid ethyl ester (21 g, 89 mmol) obtained in Reference Example 25 at 50° C. over a period of time for 30 minutes. The mixture is heated under reflux for 30 minutes, and thereto are added successively water (6 ml), a 15% sodium hydroxide (6 ml) and water (18 ml) in order to quench the reaction. The reaction solution is filtered to remove the insoluble materials, and the filtrate is concentrated under reduced pressure. The residue is purified by silica gel column chromatography (eluent: ethyl acetate) to give the title compound (17.5 g) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555557B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-c21d401ceed7477194f4fb12550fec18 |
| Source note | uspto-grants-2003_04 |