HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 1-(3-chloropropyl)-5-methyl-1H-quinolin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 1-(3-Chloropropyl)-5-methyl-3,4-dihydroquinolin-2(1H)-one | HCID 19027733 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-(3-chloropropyl)-5-methyl-1H-quinolin-2-one | HCID 17956068 | 66.1% |
Reaction Steps
A microwave vial was charged with 1-(3-chloropropyl)-5-methyl-3,4-dihydro-1H-quinolin-2-one (0.081 g, 0.34 mmol), DDQ (0.116 g, 0.51 mmol), dioxane (2 mL) and sealed. After microwave irradiation, 175° C., 10 min, the reaction was diluted with EtOAc (50 mL), washed with sat aqueous NaHCO3 (2×15 mL) and the organic phase was dried (Na2SO4), filtered, concentrated under reduced pressure and the residue was purified with prep RP-HPLC to yield the crude title compound (0.053 g), which was used without further purification. HPLC-MS (ammonium acetate) [M+H]+=236.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07307075B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-04453a3f306c4746bfbfc29724b0ca39 |
| Source note | uspto-grants-2007_12 |