HRID1084885
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1.69 ml (20.9 mmol) of pyridine and 1.5 ml (20.9 mmol) of thionyl chloride are added successively at -5° C. to 5 g (13.9 mmol) of the compound from Example 4 dissolved in 100 m of dry tetrahydrofuran and the mixture is stirred for 15 minutes at the same temperature. The mixture is diluted using ethyl acetate and extracted several times using saturated sodium hydrogen carbonate solution, and the organic phases are dried over magnesium sulphate and concentrated in vacuo. The residue is chromatographed on a column (silica gel 70-230 mesh, in petroleum ether/ethyl acetate 95:5).
WORKUP
后处理
- additionThe mixture is diluted
- extractionextracted several times
- dry with materialthe organic phases are dried over magnesium sulphate
- concentrationconcentrated in vacuo
- customThe residue is chromatographed on a column (silica gel 70-230 mesh, in petroleum ether/ethyl acetate 95:5)