HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 59234713, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | KR-33494 | HCID 25009726 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Oxalyl chloride | HCID 65578 | — |
| Product | HCID 59234713 | HCID 59234713 | 19% |
Reaction Steps
113 mg (0.3 mM) of the compound obtained in Example 23 was dissolved in 1 ml of tetrahydrofuran to which 60 μl (0.7 mM) of oxalyl chloride was added dropwise, and the resulting mixture was stirred under a nitrogen atmosphere for 30 minutes. Subsequently, 70 μl of NH4OH was added thereto, and the resulting mixture was stirred under a nitrogen atmosphere for 1 hour. The solvent was distilled off under reduced pressure, and the resultant was extracted with ethyl acetate and brine. The organic solvent layer was dried over anhydrous sodium sulfate, filtered, and then distilled under reduced pressure. The resulting impure compound was purified by column chromatography (hexane:ethyl acetate=2:1), to obtain 21 mg (19%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939550B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-41f7026ebe40465ba8d1fe9a21c03d8c |
| Source note | uspto-grants-2011_05 |