HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 18378553, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Hydride | HCID 166653 | — |
| Reactant | HCID 18378674 | HCID 18378674 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18378553 | HCID 18378553 | 86.2% |
Reaction Steps
A solution of 2,3,4,5-tetrahydro-1H-pyrido[3,4-b]azepin-2-one (470 mg) in tetrahydrofuran (20 ml) was treated with lithium aluminum hydride (990 mg) and stirred at room temperature for 30 minutes. The excess hydride was decomposed with 28% ammonium hydroxide at 0° C. The resulting mixture was filtered through a bed of Celite and the Celite was washed with tetrahydrofuran, and the filtrate was concentrated. The residual aqueous layer was extracted with chloroform, dried over sodium sulfate, concentrated and purified by silica gel column chromatography (SiO2; 20 g, 1% methanol in chloroform) to give 2,3,4,5-tetrahydro-1H-pyrido[3,4-b]azepine (370 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06495542B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-244ca721b99744a59cacfe30bd146b4a |
| Source note | uspto-grants-2002_12 |