HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylmethylenammonium chloride → 2-Dimethylaminomethyl-9-hydroxy-4H-1,3-thiazolo[5,4-c]isoquinolin-5-one hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylmethylenammonium chloride | HCID 11051579 | — |
| Reactant | 9-Hydroxy-4H-1,3-thiazolo[5,4-c]isoquinolin-5-one | HCID 58016060 | — |
| Solvent | acetonitrile N,N-dimethylformamide | HCID 21891449 | — |
| Product | 2-Dimethylaminomethyl-9-hydroxy-4H-1,3-thiazolo[5,4-c]isoquinolin-5-one hydrochloride | HCID 67076431 | 13% |
Reaction Steps
To a solution of 9-hydroxy-4H-1,3-thiazolo[5,4-c]isoquinolin-5-one in DMF/acetonitrile (3 ml, 1:2) was added dimethyl-methylene-ammonium chloride (0.043 g, 0.46 mmol) and the resulting mixture was refluxed under Ar for 42 hours. After cooling and concentration, the residue was purified via flash chromatography on SiO2 to give the title compound (0.008 g, a 13% yield) as solid. m.p.>250° C.; 1H NMR (400 MHz, DMSO) δ 2.36 (s, 6H, N(CH3)2), 3.93 (m, 2H, CH2N), 7.24 (d, 1H, Ar), 7.44 (t, 1H, Ar), 7.74 (d, 1H, Ar), 10.23 (s, 1H, OH), 12.30 (s, 1H, NH); 13C NMR (100.6 MHz, DMSO) δ 46.83, 61.38, 119.94, 120.56, 121.00, 126.83, 129.95, 131.75, 137.39, 154.41, 162.54.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08906935B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-2d45f6d80c2d44b4b583011d4b5a5125 |
| Source note | uspto-grants-2014_12 |