HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl 2,2-dimethyl-3-oxobutanedioate → HCID 178500127, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl 2,2-dimethyl-3-oxobutanedioate | HCID 85519062 | — |
| Reactant | HCID 178432595 | HCID 178432595 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178500127 | HCID 178500127 | 19.1% |
Reaction Steps
615 mg (3.27 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 13 ml of ethanol and heated to reflux. Subsequently, 652 mg (2.18 mmol) of 1-(2-fluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 13 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 30:70→100:0). 182 mg of the target compound were obtained (19% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09023849B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-ebe7556610ab4032a8de71bef91e7ac9 |
| Source note | uspto-grants-2015_05 |