HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 18726777, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 22614844 | HCID 22614844 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18726777 | HCID 18726777 | 166.7% |
Reaction Steps
2,4-Bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulphide (Lawesson's reagent) (19.5 g, 48.2 mmol) was added to a solution of 6,7-dichloro-2,3-dimethoxy-5-methoxyacetamidoquinoxaline (27 g, 78 mmol) in tetrahydrofuran (480 ml) and the mixture was stirred for 18 hours at room temperature, then evaporated under reduced pressure. The residue was purified by flash chromatography on silica gel by gradient elution using hexane:dichloromethane (1:1 changing to 1:4, by volume) as the eluent to give 6,7-dichloro-2,3-dimethoxy-5-methoxythioacetamidoquinoxaline (29.1 g, >100%) as a white solid, mp 198-200° C., containing a minor impurity.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06333326B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-a807ff263e9a47199f9ba1469de65835 |
| Source note | uspto-grants-2001_12 |