HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl 2,2-dimethyl-3-oxobutanedioate → HCID 178500124, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl 2,2-dimethyl-3-oxobutanedioate | HCID 85519062 | — |
| Reactant | HCID 178512734 | HCID 178512734 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178500124 | HCID 178500124 | 15.6% |
Reaction Steps
218 mg (1.13 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 5 ml of ethanol and heated to reflux. Subsequently, 205 mg (0.75 mmol) of 1-(2-fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazole-3-carboximidohydrazide suspended in 5 ml of ethanol were added and the mixture was boiled under reflux overnight. After cooling, the mixture was filtered, the filtercake was washed with a little ethanol and the filtrate was concentrated. The residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 20:80→100:0). 48 mg of the target compound were obtained (purity 54%; 8% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09023849B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-09880d91a89c4072bd0e517a4373b864 |
| Source note | uspto-grants-2015_05 |