HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 71765537, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 71765536 | HCID 71765536 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71765537 | HCID 71765537 | — |
Reaction Steps
A solution of 18.9 mg (0.055 mmol) 2-chloromethyl-6-(4-trifluoromethoxy-phenyl)-5H-pyrazolo[1,5-a]pyrazin-4-one in 0.5 ml THF is flushed with nitrogen. 3.5 mg (0.092 mmol) Lithiumaluminiumhydride is added and the reaction mixture is stirred for 5 hours at room temperature. Then 1 ml THF, 3.5 μl water, 3.5 μl 15% aqueous NaOH solution and 10.5 μl water are added successively. The resulting suspension is stirred for 30 minutes at room temperature. The precipitate is filtered off and washed with THF and ethanol. The filtrate is evaporated and purified by preparative HPLC to give 2-methyl-6-(4-trifluoromethoxy-phenyl)-5H-pyrazolo[1,5-a]pyrazin-4-one as colourless crystals; HPLC/MS 2.53 min (B), [M+H] 310;
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09120805B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-2056aa1e3a7d4d1781ee29e2e9405795 |
| Source note | uspto-grants-2015_09 |