HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 53713758, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 12782772 | HCID 12782772 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 53713758 | HCID 53713758 | 7% |
Reaction Steps
Methyl 5-methylsulphanylnicotinate (916 mg, 5 mmol) is dissolved in 150 mL of diethyl ether, admixed at 0° C. with lithium aluminium hydride (660 mg, 18 mmol) and subsequently stirred at room temperature for 90 minutes. The reaction is discontinued by addition of 10% ammonium chloride solution at 0° C. The batch is diluted with water and the aqueous phase is extracted with ether. Drying of the organic phase over sodium sulphate, concentrating the solvent and also chromatographic purification of the residue (silica gel, n-hexane/ethyl acetate: 50→100% ethyl acetate) gives the desired product in 7% yield (50 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07863283B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-357f3124678a4c5495a2f53f72e8c1f8 |
| Source note | uspto-grants-2011_01 |