反応 #2857

反応方程式

5H-Thieno[3,2-c]pyridin-4-one

phosphorous oxy chloride

→

title compound

4-Chloro-thieno[3,2-c]pyridine

反応条件

後処理

1. 1
   濃縮the solution is concentrated
2. 2
   workup.DISSOLUTIONThe residue is dissolved in CH2 Cl2
3. 3
   洗浄The resulting solution is washed with water and saturated NaCl
4. 4
   乾燥The organic layer is dried over MgSO4
5. 5
   ろ過filtered
6. 6
   濃縮concentrated
7. 7
   その他The crude product is purified by column chromatography
8. 8
   洗浄eluting with a gradient of 40% CH2Cl2 /hexanes to 60% CH2Cl2 /hexanes

実験手順

5H-Thieno[3,2-c]pyridin-4-one (1.0 g, 6.62 mmol) is dissolved in 30 mL of phosphorous oxy chloride. The solution is heated to 100° C. After 4 h, the solution is concentrated. The residue is dissolved in CH2 Cl2. The resulting solution is washed with water and saturated NaCl. The organic layer is dried over MgSO4, filtered and concentrated. The crude product is purified by column chromatography eluting with a gradient of 40% CH2Cl2 /hexanes to 60% CH2Cl2 /hexanes. The title compound (1.0 g, 5.8 mmol) is obtained as a white solid.

出典