HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59526152, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl bromoacetate | HCID 60984 | — |
| Reactant | HCID 59526009 | HCID 59526009 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59526152 | HCID 59526152 | — |
Reaction Steps
5-[2,6-Difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-[(6-oxo-1,6-dihydropyridazin-3-yl)amino]thiophene-3-carboxamide (Example 578 Step 3) (50 mg, 0.12 mmol), K2CO3 (18.70 mg, 0.14 mmol) and methyl bromoacetate (0.012 mL, 0.13 mmol) were stirred in DMF (1 mL) at 80° C. overnight. The reaction mixture was cooled to room temperature, water was added and the reaction mixture was extracted into EtOAc (×2). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. Purification of the residue by silica gel column chromatography (0-15% MeOH—CHCl3) gave the title compound as a yellow solid after triturating in DCM.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367706B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-a62e55b8ec07420e87886a4f2b09a83e |
| Source note | uspto-grants-2013_02 |