反応 #62070

反応方程式

[6-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-thianthren-2-yl]-carbamic acid tert-butyl ester

2-chloro-6-morpholin-4-yl-pyran-4-one

2-Chloro-6-morpholin-4-yl-pyran-4-one

K2CO3

→

title compound

収率 127.4%

[6-(6-Morpholin-4-yl-4-oxo-4H-pyran-2-yl)-thianthren-2-yl]-carbamic acid tert-butyl ester

収率 127.4%

溶媒

1,4-dioxane

反応条件

後処理

1. 1
   workup.ADDITIONwas then added The dark brown mixture
2. 2
   濃縮The reaction mixture was concentrated in vacuo and water (100 ml)
3. 3
   workup.ADDITIONwas added
4. 4
   ろ過The brown solid was filtered
5. 5
   洗浄washed with water
6. 6
   その他dried overnight in a vacuum desiccator
7. 7
   その他was used without any further purification

実験手順

[6-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-thianthren-2-yl]-carbamic acid tert-butyl ester (8.34 g, 18.24 mmol), 2-chloro-6-morpholin-4-yl-pyran-4-one (3)(4.72 g, 21.89 mmol) and grinded K2CO3 (5.04 g, 36.48 mmol) were dissolved in dry 1,4-dioxane (100 ml). The mixture was degassed for 15 minutess and Pd(PPh3)4 (1.02 g, 0.91 mmol) was then added The dark brown mixture was heated to 100° 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, washed with water, dried overnight in a vacuum desiccator and was used without any further purification to give the title compound (11.87 g). m/z (LC-MS, ESP), RT=4.61 min, (M++1)=511.2

出典