Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 11106054 | HCID 11106054 | — |
| Reactant | HCID 58515525 | HCID 58515525 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58515524 | HCID 58515524 | 38.6% |
Reaction Steps
An amount of 1 g (4.254 mmol) of 2,3-dichloro-6,7,8,9-tetrahydropyridazino[1,2-a]pyridazine-1,4-dione (II-1) is introduced in 20 ml of absolute tetrahydrofuran. Subsequently 0.869 g (4.254 mmol) of disodium (Z)-1,2-dicyanoethene-1,2-bis(thiolate) and 2 ml of water are added and the mixture is stirred at 40° C. for 18 hours. It is filtered with suction and extracted with methylene chloride and water, and the extract is dried and concentrated. Chromatography on silica gel (cyclohexane/ethyl acetate 0-100%) gives 0.5 g (99% purity, 38.3% of theory) of 5,12-dioxo-5,7,8,9,10,12-hexahydro[1,4]dithiino[2,3-d]pyridazino[1,2-a]pyridazine-2,3-dicarbonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08530387B2 |
|---|
| Source dataset | uspto-grants-2013_09 |
|---|
| ORD ID | ord-a6a1db00c0a14959b5893317cc088c13 |
|---|
| Source note | uspto-grants-2013_09 |
|---|