HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 58474361, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 58474929 | HCID 58474929 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58474361 | HCID 58474361 | 93.8% |
Reaction Steps
To a solution of 152 (150 mg, 0.311 mmol) in MeOH (20 mL) was added ammonium chloride (33.3 mg, 0.622 mmol) in water (5 mL) and zinc powder (81 mg, 3.01 mmol) and the reaction mixture was heated to reflux for 3 hours. The mixture was cooled to RT then filtered and the filtrate was concentrated under reduced pressure. The residue was dissolved in DCM and washed with water. The organic phase was collected, dried over anhydrous Na2SO4, filtered and concentrated to afford title compound 153 (132 mg, 92% yield) that was used directly in the next step with no additional purification. MS (m/z)=453.2 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08906852B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-07445b9bb190473caa0b2447e95b5b2f |
| Source note | uspto-grants-2014_12 |