HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → HCID 89768198, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | Ethyl 4-methyl-2-(trifluoromethyl)pyrimidine-5-carboxylate | HCID 10609709 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 89768198 | HCID 89768198 | 97.2% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a mixture of ethyl 4-methyl-2-(trifluoromethyl)pyrimidine-5-carboxylate (122.4 mg) in toluene (5.1 mL) was added diisobutylaluminum hydride (1.0 mol/L in hexane, 1.150 mL) at 0° C. The mixture was stirred at 0° C. under nitrogen atmosphere for 2.5 h, and then at room temperature for 2 h. To the mixture was added diisobutylaluminum hydride (1.0 mol/L in hexane, 0.58 mL) again at 0° C. and the mixture was stirred at 0° C. for 2 h. To the mixture was added sodium sulfate decahydrate (556 mg), and the mixture was stirred at room temperature overnight. The mixture was filtered through on the pad of Celite®. The filtrate was concentrated in vacuo to give the title compound (97.6 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238639B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-464c8003ef5d4dfa89dd122143c0839a |
| Source note | uspto-grants-2016_01 |