反应详情

温度

130 °C

(4-Amino-2,6-dimethyl-phenyl)-carbamic acid propyl ester (84 mg) and 5-chloro-thiophene-2-carbaldehyde (48 uL) were dissolved in methanol (3 mL) and heated to 130° C. for 5 minutes in a sealed microwave process vial. Sodium cyanoborohydride (95 mg) was added and the reaction mixture was heated to 130° C. for 5 minutes in a sealed microwave process vial, followed by addition of water/brine (1:1, 3 mL). The product was extracted with ethyl acetate (3×3 mL) and the combined organic phases were washed with brine (5 mL), dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 66 mg (49% yield) of the title compound as an oil. LC-MS (m/z) 353 (MH+); tR=3.06, (UV, ELSD) 87%, 87%.

1. temperaturethe reaction mixture was heated to 130° C. for 5 minutes in a sealed microwave process vial
2. extractionThe product was extracted with ethyl acetate (3×3 mL)
3. washthe combined organic phases were washed with brine (5 mL)
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash chromatography