HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-(1-Azidotridecyl)-5-trimethylsilylfuran → 3-(1-Aminotridecyl)-5-trimethylsilylfuran
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-(1-Azidotridecyl)-5-trimethylsilylfuran | HCID 19019847 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-(1-Aminotridecyl)-5-trimethylsilylfuran | HCID 15037077 | — |
Reaction Steps
Lithium aluminum hydride (a 1M solution in tetrahydrofuran; 1.1 ml, 1.1 mmol) was added dropwise to a solution of 3-(1-azidotridecyl)-5-trimethylsilylfuran (334 mg, 0.92 mmol) in tetrahydrofuran at room temperature. After one hour at room temperature, the excess hydride was destroyed by adding acetone slowly to the mixture with cooling. Sodium sulfate (ca. 0.5 g) was added and the mixture was extracted thoroughly with ethyl acetate. Evaporation of the dried (magnesium sulfate) extracts gave an oil, which was purified by flash chromatography on silica using 5% methanol/dichloromethane containing 0.2% triethylamine. Fractions with Rf of about 0.18 on evaporation gave the title amine as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05298633 |
| Source dataset | uspto-grants-1994_03 |
| ORD ID | ord-e5e84b24cc6f4795b20e7cb4e14446e1 |
| Source note | uspto-grants-1994_03 |