反应详情

Thionylchloride (2.96 ml, 1.3 eq.) was added dropwise under ice-cooling to compound 643 (9.09 g, 32 mM) dissolved in chloroform (30 ml), and stirred at room temperature for 2 hours. Dilute aqueous K2CO3 was added to the reaction mixture, which mixture was then extracted twice with chloroform, dried with anhydrous sodium sulfate and concentrated in vacuo. The residue was charged on a column of silica-gel (C-200, 100 g) packed with chloroform and eluted with chloroform to obtain compound 644 (7.55 g, yield: 78.0%).

1. extractionwas then extracted twice with chloroform
2. dry with materialdried with anhydrous sodium sulfate
3. concentrationconcentrated in vacuo
4. additionThe residue was charged on a column of silica-gel (C-200, 100 g)
5. washeluted with chloroform