HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 86644284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 86644285 | HCID 86644285 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86644284 | HCID 86644284 | 85.2% |
Reaction Steps
Compound 14c (17.3 g) was dissolved in tetrahydrofuran (180 ml) and methanol (180 ml), and iron powder (19.1 g) was added thereto. An ammonium chloride aqueous solution (1.67 mol/l, 110 ml) was added to the reaction mixture while refluxing under heating. The obtained mixture was refluxed under heating for 1 hour. After the mixture was allowed to cool, the iron powder was removed by Cerite filtration. Ethyl acetate and purified water were added to the filtrate, and extraction and washing were carried out. The organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was recrystallized with n-heptane to obtain Compound 14d (13.0 g, 85%) as an opalescent solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07855300B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-ea592dcb1b17406b8b18ebbc79950cf7 |
| Source note | uspto-grants-2010_12 |