HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → [3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-4-yl]methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate | HCID 9877977 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | [3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-4-yl]methanol | HCID 23076503 | 92.7% |
Reaction Steps
To a solution of ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate (15.00 g) in tetrahydrofuran (150 mL) was added lithium aluminum hydride (1.93 g) at 0° C., and the mixture was stirred at room temperature for 1 hr. Sodium sulfate 10 hydrate (21.03 g) and hexane (100 mL) were added to the reaction mixture, and the mixture was stirred at room temperature for 1 hr. The precipitate was removed by filtration and the filtrate was concentrated. The obtained crystals were collected by filtration to give [3-methyl-1-(2-pyridyl)-1H-pyrazol-4-yl]methanol (11.38 g). The crystals were recrystallized from acetone-hexane. melting point: 116-117° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07238716B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-2f2c036c73ee4a1984c52435a441672d |
| Source note | uspto-grants-2007_07 |