HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1'-Thiocarbonyldiimidazole → HCID 89690173, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| Reactant | rac-Tert-butyl 7,8-dihydroxy-2,3-di-p-tolyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate | HCID 66665909 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 89690173 | HCID 89690173 | — |
Reaction Steps
tert-Butyl 7,8-di hydroxy-2,3-d i-p-tolyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (step 2) (1.28 g, 2.86 mmol) was dissolved in tetrahydrofuran (50 ml). 1,1′-Thiocarbonyl diimidazole (1.019 g, 5.72 mmol) was added and the solution heated at reflux for 3 h. The reaction mixture was cooled to room temperature and evaporated to dryness. Water and DCM (300 ml) were added. The organic layer was separated and evaporated to dryness. Ethyl acetate (5 ml) was added to the dark residue and the resulting solid filtered off. The solid was washed twice with EtOAc (5 ml) to afford the titled compound;
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115129B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-8238023a7acf4b1f9fb972d1f5faa036 |
| Source note | uspto-grants-2015_08 |