HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → (2-Chloropyridin-4-yl)methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Methyl 2-chloropyridine-4-carboxylate | HCID 2736842 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (2-Chloropyridin-4-yl)methanol | HCID 7062237 | 94% |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
Methyl 2-chloropyridine-4-carboxylate (2.50 g, 14.60 mmol) was dissolved in anhydrous THF (50 mL) and this solution was cooled to −78° C. under N2 atmosphere. Diisobutylaluminium hydride 1.0 M in hexanes (63.3 mL, 63.30 mmol) was added dropwise stabilizing the temperature between −50° C. and −70° C. The reaction mixture was stirred 1.5 h at −78° C. and allowed to stand at room temperature for 3 h. A solution of aqueous 10% NH4Cl was slowly added and the mixture was extracted with ethyl acetate (3×300 mL). The combined organic layers were washed with water (3×20 mL), brine (2×20 mL), dried over MgSO4, filtered and evaporated. (2-Chloropyridin-4-yl)methanol SLA 07152 was obtained as a yellow oil (1.97 g, 94% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431599B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-0f24c280a9cb44f5af86d78f4dec8724 |
| Source note | uspto-grants-2013_04 |