HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 66852447, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 58105210 | HCID 58105210 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66852447 | HCID 66852447 | 41.6% |
Reaction Steps
To a suspension of 420 mg of LiAlH4 in 20 mL of THF, the solution of 1.9 g of 3-[6-(t-butyldimethylsilanyl-oxymethyl)pyridin-2-yl]-1-morpholin-4-ylpropan-1-one in 30 mL of THF was added dropwise at ice temperature. After the reaction mixture was stirred at room temperature for 3 hours, the excess LiAlH4 was quenched with water, and the solution was filtrated through Hyflo Super-Cel (Nacalai Tesque) and partitioned. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate. After removing the solvent under reduced pressure, the residue was purified by chromatography on silica gel (methylene chloride-ethanol 40:1) to give 760 mg of 4-{3-[6-(t-butyldimethylsilanyloxymethyl)pyridin-2-yl]propyl}morpholine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989446B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-b45a225d5a674da8a82b0193c3c9bc3d |
| Source note | uspto-grants-2011_08 |