HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → [4-Methyl-6-oxopyridazin-1(6H)-yl]acetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | ethyl [4-methyl-6-oxopyridazin-1(6H)-yl]acetate | HCID 77231410 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | [4-Methyl-6-oxopyridazin-1(6H)-yl]acetic acid | HCID 66939440 | — |
Reaction Steps
To ethyl [4-methyl-6-oxopyridazin-1(6H)-yl]acetate (0.575 g, 2.93 mmol) in tetrahydrofuran (3 mL), methanol (2 mL) and water (2 mL) was added 1 N lithium hydroxide solution (2.9 mL). The reaction mixture was stirred at ambient temperature for 1.5 h. After neutralized with trifluoro acetic acid, the reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-45% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient). The pure fractions were lyophilized overnight to yield the title compound. LC/MS 169.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247415B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-e372c6c011c44ef88c95a22c13288876 |
| Source note | uspto-grants-2012_08 |