HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonyl chloride → HCID 1811360, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonyl chloride | HCID 7369 | — |
| Reactant | 3-hydroxy-1,2,3-benzotriazin-4(3H)-one | HCID 73026 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 1811360 | HCID 1811360 | 89.6% |
Reaction Steps
In water (20 ml) are dissolved 4-oxo-3,4-dihydro-3-hydroxy-1,2,3-benzotriazine (2.4 g) and sodium hydrogen carbonate (1.3 g), and thereto is added a solution of benzenesulfonyl chloride (2.65 g) in ethyl acetate (20 ml) under ice-cooling and the mixture is stirred for 2 hours. The precipitated crystals are separated by filtration. The ethyl acetate layer is separated from the filtrate and concentrated. The resulting crystals are separated by filtration and combined with the crystals obtained above. The crystals are washed with ether, dried and then recrystallized from benzene to give 4-oxo-3,4-dihydro-3-benzene-sulfonyloxy-1,2,3-benzotriazine (4.0 g), melting point: 132°-134° C. Infrared spectrum: 1705, 1390, 1195 cm-1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04242507 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-8b7d490f22cd4969ae8a5a653fb72c15 |
| Source note | uspto-grants-1980_12 |