HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → (2-Chloro-4,5-difluorophenyl)methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | Methyl 2-chloro-4,5-difluorobenzoate | HCID 22149760 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Lithium aluminum hydride | HCID 28112 | — |
| Product | (2-Chloro-4,5-difluorophenyl)methanol | HCID 720763 | — |
Reaction Steps
To 2-chloro-4,5-difluoro-benzoic acid methyl ester (119, 5.70 g, 0.0276 mol) in tetrahydrofuran (120.0 mL), 1.00 M of lithium tetrahydroaluminate in tetrahydrofuran (30.0 mL) was added slowly under an atmosphere of nitrogen. The reaction was stirred at room temperature for 4 hours, followed by adding sodium sulfate decahydrate. After 30 minutes, the reaction mixture was filtered, concentrated and purified with silica gel column chromatography eluting with 8% methanol in dichloromethane to give a white solid (120, 4.20 g, 85.2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07872018B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-1a335e479b1048a48dc2c4850ced366c |
| Source note | uspto-grants-2011_01 |