HRID1193342
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
2 M HCl (13.6 ml) was added to a solution of 4-(1,4-dioxaspiro[4.5]decan-8-yl)pyridine (3.0 g, 13.6 mmol, 1 eq) in THF (136 ml), and stirring was carried out for 3 h at RT. The solvent was removed under reduced pressure. The residue was diluted with water (50 ml) and rendered basic with solid sodium hydrogen carbonate. Then extraction with ethyl acetate (2×100 ml) was carried out. The combined organic phases were washed with water (80 ml), dried over sodium sulfate and concentrated under reduced pressure. The desired product was used in the next step without being purified further. Yield: 69% (1.65 g, 9.42 mmol).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- additionThe residue was diluted with water (50 ml)
- extractionThen extraction with ethyl acetate (2×100 ml)
- washThe combined organic phases were washed with water (80 ml)
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customwithout being purified further