HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → HCID 117840022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 117840421 | HCID 117840421 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 117840022 | HCID 117840022 | 38.8% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of lithium aluminium hydride (300 mg) in tetrahydrofuran (20 mL) was added dropwise a solution of ethyl 4-(4-nitrophenyl)tetrahydro-2H-pyran-4-carboxylate (1.0 g) obtained in Step A of Example 151 in tetrahydrofuran (10 mL) at −78° C., and the mixture was stirred at 0° C. for 1 hr. To the reaction mixture was added sodium sulfate decahydrate, and the mixture was stirred at room temperature for 2 hr. The insoluble substance was removed by filtration through Celite, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (330 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187453B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-7f6056a03d994fdb9e95cfc962631a08 |
| Source note | uspto-grants-2015_11 |