반응 #2857

반응 방정식

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

phosphorous oxy chloride

→

title compound

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

반응 조건

후처리

1. 1
   농축the solution is concentrated
2. 2
   workup.DISSOLUTIONThe residue is dissolved in CH2 Cl2
3. 3
   세척The resulting solution is washed with water and saturated NaCl
4. 4
   건조The organic layer is dried over MgSO4
5. 5
   여과filtered
6. 6
   농축concentrated
7. 7
   기타The crude product is purified by column chromatography
8. 8
   세척eluting with a gradient of 40% CH2Cl2 /hexanes to 60% CH2Cl2 /hexanes

실험 절차

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.

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