HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 68628529, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 66631925 | HCID 66631925 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 68628529 | HCID 68628529 | 90% |
Reaction Steps
A mixture of intermediate 62 (180 mg, 0.41 mmol), Fe (70 mg, 1.23 mmol) and ammonium chloride (25 mg, 0.41 mmol) was dissolved in EtOH and H2O, and the solution was heated to reflux and stirred overnight. The solution was filtered, diluted with water, and then extracted with DCM. The combined organic layers were washed with saturated aq NaHCO3, brine, dried over anhydrous Na2SO4, and concentrated in vacuo to give 5-(4-(4-(2,3-dichlorophenyl)piperazin-1-yl)butoxy)-2-methylaniline (intermediate 63) (150 mg, 90%) as a yellow solid. HPLC: 99%, RT 3.197 min. MS (ESI) m/z 407.9 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156822B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-5e7a23b8023243b7b09ec26e6e65f842 |
| Source note | uspto-grants-2015_10 |