Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium | HCID 223 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | HCID 10867629 | HCID 10867629 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 53729251 | HCID 53729251 | 48.5% |
Reaction Steps
Lithium aluminum hydride (2.2 g) was added to a THF (200 ml) solution of the compound 324-1 (12.4 g), while the solution was stirred under cooling on ice. The obtained mixture was stirred at room temperature for 3 hours. Ice was added by portions to the reaction solution, and thereby excessive lithium aluminum hydride was decomposed. Thereafter, a small amount of 27% ammonium aqueous solution and Celite were added to the residue, and the obtained mixture was stirred at room temperature for 20 minutes. Magnesium sulfate was added to the reaction solution, and the mixture was filtered. The filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-heptane/ethyl acetate=1:0 to 3:1), so as to obtain the title compound (5.23 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268848B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-a7770ce7dc6e48118010868f51a992ae |
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| Source note | uspto-grants-2012_09 |
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