HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 22731423, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 22731415 | HCID 22731415 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 22731423 | HCID 22731423 | 98% |
Reaction Steps
Under cooling with ice, a solution of methyl ester of 5-tert-butyl-4-sulfamoyl-furan-2-carboxylic acid (1.90 g) in THF (20 ml) was added dropwise to a suspension of lithium aluminum hydride (0.55 g) in THF (10 ml) over 35 min., followed by stirring for 2 hours. The reaction mixture was diluted with n-hexane, mixed with saturated aqueous ammonium chloride (5 ml) and filtered on Celite, being washed with ethyl acetate. The filtrate was dried over magnesium sulfate and evaporated to remove the solvent; the thus obtained residue was subjected to silica gel column chromatography (developing solvent: n-hexane:ethyl acetate=1:1) to give the titled compound (1.66 g, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06720433B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-af516833b0bc497db0cb5661eb807e8e |
| Source note | uspto-grants-2004_04 |