反应详情

A solution of 4-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4H-isothiazol-3-yl]-2-methyl-benzamide (200 mg) and N,N-Dimethylformamide dimethylacetal (4 mL) was refluxed under argon for one hour then the solution was concentrated in vacuo. The residue was dissolved in 1,4-dioxane (2 mL) and a solution of O-methylhydroxylamine hydrochloride (2.8 eq.) and sodium hydroxide (6 eq.) in water (1.6 mL) and acetic acid (1.6 mL) was added. The solution was stirred at rt for 10 minutes. It was then quenched by addition of water and extracted with methyl tert-butyl ether. The combined organic extracts were washed with brine, dried over magnesium sulfate and evaporated. Flash Chromatography eluting with Cyclohexane:EtOAc afforded 243 mg of the title compound.

1. concentrationthe solution was concentrated in vacuo
2. dissolutionThe residue was dissolved in 1,4-dioxane (2 mL)
3. customIt was then quenched by addition of water
4. extractionextracted with methyl tert-butyl ether
5. washThe combined organic extracts were washed with brine
6. dry with materialdried over magnesium sulfate
7. customevaporated
8. washFlash Chromatography eluting with Cyclohexane