HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione Methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | (9S)-9-ethyl-3-hydroxy-6-nitro-7,8,9,10-tetrahydropyrido[3,4-f]quinoxalin-9-ium-2-olate | HCID 10266209 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione Methanesulfonate | HCID 22742464 | 92% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
The product from Example 74 was suspended in 300 mL dimethylformamide and 1 mL of 3 N methanesulfonic acid added. The suspension was warmed to 100° C. The colour changed from orange to yellow and all of the solid dissolved. Solvent was evaporated in vacuo, the yellow residue washed with acetone and then dried under vacuum over P2O5 to give the title compound (0.73 g, 92% yield) mp=302-304° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06703391B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-da20f6b9c3c44a1780128c8672b4caa0 |
| Source note | uspto-grants-2004_03 |