HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → N-{1-[(5-Amino-1,3,4-oxadiazol-2-yl)methyl]-2-oxo-1,2,3,4-tetrahydroquinolin-3-yl}-2-chloro-6H-thieno[2,3-b]pyrrole-5-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Cyanogen Bromide | HCID 10476 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 2-chloro-N-[1-(2-hydrazino-2-oxoethyl)-2-oxo-1,2,3,4-tetrahydroquinolin-3-yl]-6H-thieno[2,3-b]pyrrole-5-carboxamide | HCID 58721826 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | N-{1-[(5-Amino-1,3,4-oxadiazol-2-yl)methyl]-2-oxo-1,2,3,4-tetrahydroquinolin-3-yl}-2-chloro-6H-thieno[2,3-b]pyrrole-5-carboxamide | HCID 10026388 | 20% |
Reaction Steps
1,4-Dioxane (5 mL), 2-chloro-N-[1-(2-hydrazino-2-oxoethyl)-2-oxo-1,2,3,4-tetrahydroquinolin-3-yl]-6H-thieno[2,3-b]pyrrole-5-carboxamide (Method 15; 300 mg, 0.72 mmol), cyanogen bromide (80 mg, 0.75 mmol) and 1,4-dioxane (2 mL) were added to a solution of Na2CO3 (77 mg, 0.72 mmol) in H2O (1.7 mL) and stirred for 18 hours. The mixture was diluted with EtOAc (50 mL) and THF (20 mL) and washed with H2O (25 mL). The organic was dried (Na2SO4), filtered and evaporated. The residue was purified by reverse phase column chromatography to give a brown solid. This was triturated with refluxing Et2O (25 mL), filtered, washed with Et2O (25 mL) then hexane (25 mL) to afford the title compound (63 mg, 20%) as a brown powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07276517B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-9e4c01fc64a2470196c0f002b0f328eb |
| Source note | uspto-grants-2007_10 |