Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 58424908 | HCID 58424908 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58424901 | HCID 58424901 | 99.3% |
Reaction Steps
Tetrahydrofuran (10.0 ml) was added to lithium aluminum hydride (125 mg, 3.30 mmol) and cooled to 0° C. The compound (457 mg, 1.32 mmol) prepared in step 7 was dissolved in tetrahydrofuran (10.0 ml) was added dropwise slowly at 0° C. and the resulting mixture was stirred at the same temperature for 1 hour. After completion, ammonium chloride aqueous solution was added and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residue was then purified by flash column chromatography (dichloromethane:methanol=10:1) to obtain the title compound (399 mg, yield: 99.2%, ivory solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08815891B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-ea3aab219296417e8d60c878a4b860a9 |
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| Source note | uspto-grants-2014_08 |
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