HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 86643630, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 67029027 | HCID 67029027 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86643630 | HCID 86643630 | 97.3% |
Reaction Steps
The crude tert-butyl 5-bromo-4-carbamoylpyridin-2-ylcarbamate (Intermediate 84, 232 mmol) was treated with Lawesson's Reagent (94 g, 232 mmol, 1 eq) and tetrahydrofuran (700 mL), the resulting mixture was heated at reflux for 1 h, then it was allowed to stir at room temperature over the weekend. The mixture was concentrated to dryness in vacuo and toluene (˜300 mL) was added. A bright yellow solid precipitated formed which was collected by filtration and washed with toluene, then dried in the vacuum oven at 50° C. for 4 h, yielding 75 g of a bright yellow solid (97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08283361B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-7ee22519fe2d4c7293ab9e4725767b91 |
| Source note | uspto-grants-2012_10 |