HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 131722260, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 10585357 | HCID 10585357 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131722260 | HCID 131722260 | — |
Reaction Steps
A solution of 1.39 g (6.1 mmol) of the nitrile obtained in Step 5 in 35 ml of THF is added dropwise to a suspension of LiAlH4 (350 mg, 9.2 mmol) in 35 ml of anhydrous THF at −20° C. under nitrogen. The mixture is stirred for 1 hour 30 before being hydrolysed with 2.3 ml of H2O, 4.6 ml of 35% sodium hydroxide solution and 4.9 ml of water. The resulting suspension is filtered and the filtrate is evaporated to yield an oil which is subjected to flash chromatography over a column: the title compound is isolated in the form of a mixture of two diastereoisomers which are separable by HPLC (Kromasil 100, 10 C18-210 mm—CH3CN/H2O/CF3COOH=170/830/5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06172097B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-796061728b464aa1a449ea390522b63e |
| Source note | uspto-grants-2001_01 |