Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 86606998 | HCID 86606998 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57982477 | HCID 57982477 | 220.3% |
Reaction Steps
To a stirred solution of tert-butyl (2-carbamoyl-5-(2,4-dichlorophenyl)-7-methylimidazo[1,2-a]pyrimidin-6-yl)methylcarbamate (intermediate for Example 62, 150 mg, 0.33 mmol) in THF (10 mL) was added Lawesson's reagent (202 mg, 0.50 mmol). After heating to 65° C. for 20 h, the reaction mixture was poured into H2O (5 mL). The resulting mixture was extracted with EtOAc and the organic layer was washed with satd aq NH4Cl and brine prior to drying over MgSO4. Filtration, concentration under reduced pressure afforded crude tert-butyl (2-carbamothioyl-5-(2,4-dichlorophenyl)-7-methylimidazo[1,2-a]pyrimidin-6-yl)methylcarbamate (339 mg, 100% crude yield) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07635699B2 |
|---|
| Source dataset | uspto-grants-2009_12 |
|---|
| ORD ID | ord-5c137824ea394bcf87b613e0105111fc |
|---|
| Source note | uspto-grants-2009_12 |
|---|