HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium hydroxy sulfite → 5,6-Difluoro-2-(methylsulfinyl)benzo[d]thiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | 5,6-Difluoro-2-(methylsulfanyl)-1,3-benzothiazole | HCID 44820104 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | 5,6-Difluoro-2-(methylsulfinyl)benzo[d]thiazole | HCID 57748938 | 50.7% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of 240 mg (1.1 mmol) 5,6-difluoro-2-methylsulfanyl-benzothiazole in 8 mL methanol under nitrogen at 0-5° C., was added drop wise a solution of 1.019 g (1.658 mmol) oxone in 4 mL water. The reaction mixture was stirred at 0° C. for 1 h. The suspension was diluted with water (10 mL). The solid was filtered, washed with water and dissolved in dichloromethane. The solution was dried over Na2SO4, filtered, concentrated in vacuo and purified with flash column chromatography on silica eluting with a gradient formed from n-heptane and ethyl acetate to provide 130 mg (50.6%) of the title compound as white solid. MS(m/e): 234.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897627B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-4288027199d7457fbbb185a38f17e62c |
| Source note | uspto-grants-2011_03 |