HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → [3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | ethyl 3-(formylamino)-1-phenyl-1H-pyrazole-4-carboxylate | HCID 23076448 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | [3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol | HCID 69217492 | 96% |
Reaction Steps
Lithium aluminum hydride (7.50 g) was added to tetrahydrofuran (200 mL) under ice-cooling. To the obtained mixture was added dropwise a solution (100 mL) of ethyl 3-(formylamino)-1-phenyl-1H-pyrazole-4-carboxylate (20.50 g) in tetrahydrofuran, and the mixture was heated under reflux for 1.5 hrs. To the obtained mixture was added small portions of sodium sulfate decahydrate (50 g) on an ice bath, and the mixture was stirred for 2 hrs. while adding tetrahydrofuran (50 mL) as appropriate to allow stirring. Solids were filtered off and the filtrate was concentrated to give [3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol as a colorless oil (15.42 g, yield 96%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07368578B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-e787ff7a19494444a9d55a1cf4656842 |
| Source note | uspto-grants-2008_05 |