反应详情

温度

90 °C

6-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-thianthrene-2-carboxylic acid methyl ester (1.1 g, 2.83 mmol), 2-chloro-6-morpholin-4-yl-pyran-4-one (3) (0.73 g, 3.4 mmol) and K2CO3 (0.8 g, 5.66 mmol) were dissolved in dry 1,4-dioxane (7 ml). The mixture was degassed for 15 mins and Pd(PPh3)4 (0.16 g, 5 mol %) was then added The dark brown mixture was heated to 90° C. under an atmosphere of N2 for 24 hour. The reaction mixture was concentrated in vacuo and water (100 ml) was added. The brown solid was filtered and washed with water (1.23 g, 96%). m/z (LC-MS, ESP), RT=4.49 min, (M++1)=454.

1. customThe mixture was degassed for 15 mins
2. additionPd(PPh3)4 (0.16 g, 5 mol %) was then added The dark brown mixture
3. concentrationThe reaction mixture was concentrated in vacuo and water (100 ml)
4. additionwas added
5. filtrationThe brown solid was filtered
6. washwashed with water (1.23 g, 96%)