HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 83853743, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 90020202 | HCID 90020202 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 83853743 | HCID 83853743 | 83.8% |
Reaction Steps
Dissolve 4,4-difluoro-6-nitro-chromane (2.5 g, 11.6 mmol) in methanol (100 mL), add zinc powder (2.5 g, 34.8 mmol), then add dropwise a 15.5% aqueous solution of ammonium chloride (40 mL, 139 mmol), stir at room temperature for 5 hrs. Filter off the solid, add water (50 mL) to the filtrate, extract with EtOAc (50 mL×2). Combine the organic layers, wash with brine (50 mL×2), dry over anhydrous Na2SO4. Concentrate under reduced pressure to get a crude residue. Purification by chromatography (silica gel, EtOAc:PE=1:3) affords the title compound (1.8 g, 83.7%). MS: (M+1): 186.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359338B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-75b4daeb3f39417c943d8f529461b7e3 |
| Source note | uspto-grants-2016_06 |