HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → HCID 59383008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 59382925 | HCID 59382925 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59383008 | HCID 59383008 | — |
Reaction Steps
To a solution of (S)-tert-butyl 1-(methylamino)-3-(4-methylcyclohexyl)-1-oxopropan-2-ylcarbamate (1.0075 g, 3.38 mmol, 1.0 equiv) in THF (40 mL) was added 7 mL (7 mmol, 2.1 equiv) of 1.0 M LiAlH4 in THF at 0° C. under N2. The mixture was stirred at rt for 19 h and then sodium sulfate decahydrate (6.45 g, 20 mmol) was added carefully to quench excess LiAlH4. The mixture was filtered and the solid was washed with ether. After the solvents were removed in vacuo, the crude (S)-tert-butyl 1-(methylamino)-3-(4-methylcyclohexyl)propan-2-ylcarbamate (1.04 g) was used in the next step without further purification. MS ESI +ve m/z 285 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08487108B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-159d1de5dfbc4efb8ebb9ca2f35ac850 |
| Source note | uspto-grants-2013_07 |