HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → HCID 21704125, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 21704118 | HCID 21704118 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21704125 | HCID 21704125 | 106.7% |
Reaction Steps
Lithium aluminum hydride (2 g) was suspended in THF (40 ml) and a solution of 4-(4-methyl-1-oxa-4,9-diazaspiro[5,5]undecan-9-yl)benzonitrile (12 g) in THF (100 ml) was added dropwise under ice-cooling. The mixture was stirred at room temperature for 2 hr 40 min and a saturated aqueous sodium sulfate solution was added portionwise under ice-cooling. The precipitated solid was filtrated and washed with chloroform. The chloroform layer was dried over anhydrous sodium sulfate and, after drying, the solvent was evaporated under reduced pressure to give the objective 4-(4-methyl-1-oxa-4,9-diazaspiro[5,5]undecan-9-yl)phenylmethylamine (13 g), which was used in the next Starting Material Synthetic Example 185 without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06288061B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-b0d0888df5044a7a9e0849048031d59f |
| Source note | uspto-grants-2001_09 |