HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 21994557, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | N'-Hydroxycyclopropanecarboximidamide | HCID 2794666 | — |
| Reactant | HCID 19106541 | HCID 19106541 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21994557 | HCID 21994557 | 43.4% |
Reaction Steps
A mixture of ethyl 4-(N-ethyl-N-methylamino)-imidazo[1,5-a]quinoxaline-3-carboxylate (1.2 g, 4 mmol), cyclopropanecarboxamidoxime (1.4 g, 14 mmol), crushed 4 Å molecular-sieves (0.5 g), and sodium hydride (0.1 g, 60% in mineral oil) in dry DMF (20 ml) was stirred at ambient temperature for 1 h. Dichloromethane (25 ml) was added and the mixture was filtered through celite. The filtrate was evaporated and the residue was brought to crystallize by the addition of 10 ml of ethyl acetate and cooling to 0° C. The crystals was collected by filtration, rinsed with ethyl acetate and dried to give 0.58 g of the title compound, m.p. 96°-97° C. An additional amount (0.22 g) of the product was obtained from the mother liquour. (Compound 6).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05276028 |
| Source dataset | uspto-grants-1994_01 |
| ORD ID | ord-d5367b527ae84fa698623b7207b7c4a4 |
| Source note | uspto-grants-1994_01 |