Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus oxybromide | HCID 24613 | — |
| Reactant | HCID 67257898 | HCID 67257898 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58574864 | HCID 58574864 | 79% |
Reaction Steps
A mixture of dimethyl 2-((4-bromopyridin-2-ylamino)methylene)malonate (4.8 g, 15.2 mmol, 1 equiv) and POBr3 (16.1 g, 56.1 mmol, 3.7 equiv) was stirred at 80° C. for 2 h. After it was cooled to room temperature, the reaction mixture was poured into water carefully. Then the solution was adjusted pH to 8 with aq. Na2CO3 and extracted with DCM (3×200 mL). The combined organic layers were dried over Na2SO4 and concentrated to give 3.4 g of the desired product. MS (ESI): 283, 285 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08772301B2 |
|---|
| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-bbee26132a4c480ebd76c09e7dbfd2d4 |
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| Source note | uspto-grants-2014_07 |
|---|