HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → [(5-Nitro-1,2-benzisothiazol-3-yl)oxy]acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Bromoacetonitrile | HCID 11534 | — |
| Reactant | 1,2-Benzisothiazol-3(2H)-one, 5-nitro- | HCID 13186950 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | [(5-Nitro-1,2-benzisothiazol-3-yl)oxy]acetonitrile | HCID 18314467 | 71.5% |
Reaction Steps
A mixture of 5-nitro-1,2-benzisothiazol-3(2H)-one (17.5 g, 89.2 mmol) in N,N-dimethylformamide is treated with potassium carbonate (18.5 g, 134 mmol), stirred at room temperature for 30 minutes, treated with bromoacetonitrile (16.0 g, 133 mmol), stirred at room temperature overnight, and poured onto ice. The resultant aqueous mixture is acidified to pH 3 with hydrochloric acid and extracted with ethyl acetate. The combined organic extracts are washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a solid. Column chromatography of the solid using silica gel and methylene chloride gives the title product as a yellow solid (15.0 g, mp 123-124.5° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06355796B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-ebc2205637a146a382a372a2c8d1f71e |
| Source note | uspto-grants-2002_03 |