反应详情

温度

80 °C

Added 2e (15 g, 1.0 eq) and 2g (8.58 g, 1.07 eq) into a jacketed reactor of suitable size before adding ethyl acetate (225 ml, 15 vol) and diisopropylethylamine (5.43 g, 1.0 eq), then heated the mixture to reflux (75-85° C.) for 24 hours. Once the reaction was complete, the mixture was cooled to room temperature and stirred for an additional 1 hour. Precipitated solid was filtered, washed with EtOAc 2 times (45 ml, 3 vol each wash), then dried at 58° C. for 18 hours (until a LOD is achieved of less than 1%) to give 17.46 g of crude 2h (90.4% yield, 98.46% a/a) as a white crystalline solid.

1. temperatureheated the mixture
2. temperaturethe mixture was cooled to room temperature
3. customPrecipitated solid
4. filtrationwas filtered
5. washwashed with EtOAc 2 times (45 ml, 3 vol
6. washeach wash),
7. customthen dried at 58° C. for 18 hours (until a LOD