HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 19029811, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | HCID 11099521 | HCID 11099521 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19029811 | HCID 19029811 | 53.7% |
Reaction Steps
To 15.6 ml of liquid ammonia was added 28.5 mg of lithium metal at -78° C. and the mixture was stirred for 5 minutes. Then, 15.6 ml of a THF solution containing 500 mg of the compound obtained in Example 1 was slowly added dropwise. After the mixture was stirred at -78° C. for 1.5 hours, the ammonia was distilled off and the residue was diluted with water and extracted with diethyl ether. The organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated. The resulting crude product was purified by silica gel column chromatography (eluent=diethyl ether:n-hexane:chloroform=5:50:1) to provide 270 mg of the object compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05654343 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-149e219c1c0a44218a097b50dc06d18c |
| Source note | uspto-grants-1997_08 |