反应详情

温度

100 °C

To a stirred solution of 600 mg (1.65 mmol) (7-iodo-4-methoxy-benzothiazol-2-yl)-carbamic acid methyl ester in 10 ml dioxane were added 1.23 g (3.30 mmol) tri-n-butyl-(3,6-dihydro-2H-pyran-4-yl)-stannane, 28 mg (0.05 mmol) bis(dibenzylideneacetone)palladium and 61 mg (0.26 mmol) trifurylphosphine. The mixture was heated at 100° C. for 16 h and then poured onto water and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated in vacuo. Flash chromatography (1/9-1/3 ethyl acetate/hexane) afforded 200 mg [7-(3,6-dihydro-2H-pyran-4-yl)-4-methoxy-benzothiazol-2-yl]-carbamic acid methyl ester as a light brown solid. ES-MS m/e (%): 319 ([M−H], 100).

1. additionpoured onto water
2. extractionextracted three times with ethyl acetate
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. concentrationconcentrated in vacuo