HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → 1-Cyclohexyl-6-(3-formyl-1-pyrrolyl)-7-nitro-2,3(1H,4H)-quinoxalinedione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Tetrahydro-2,5-dimethoxyfuran-3-carbaldehyde | HCID 567310 | — |
| Reactant | 7-Amino-1-cyclohexyl-6-nitro-2,3(1H,4H)-quinoxalinedione | HCID 22097076 | — |
| Solvent | Dimethylformamide toluene | HCID 21735183 | — |
| Product | 1-Cyclohexyl-6-(3-formyl-1-pyrrolyl)-7-nitro-2,3(1H,4H)-quinoxalinedione | HCID 22097204 | 22% |
Reaction Steps
4 g (13 mmol) of the product 37b, 2.3 g (14 mmol) of 3-formyl-2,5-dimethoxytetrahydrofuran and a spatula tip of 4-toluenesulfonic acid in 200 ml of dimethylformamide/toluene (1:1) were refluxed with a water trap. After the reaction was complete (TLC check), the mixture was concentrated under reduced pressure, and the residue was partitioned between ethyl acetate and water. The organic phase was dried and concentrated under reduced pressure. This residue was purified by chromatography on silica gel (mobile phase: toluene/acetone/glacial acetic acid=40/20/1) to yield 1.1 g (22%) of the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05714489 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-f46f7893d50f46868cd06b6fe822a852 |
| Source note | uspto-grants-1998_02 |