HRID1984984
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
A solution of 1-(1-benzyl-piperidine-4-yl)-2-ethyl-5-fluoro-1H-indole (11.9 g) and acetic acid (4.1 ml) in methanol (250 ml) was hydrogenated for 8 h (50° C./1013 mbar). The mixture was then filtered and concentrated in vacuo. CH2Cl2 (250 ml), NaHCO3 (100 ml) and water (300 ml) were added and the mixture stirred for 10 min. The organic layer was extracted with CHCl3 and this was dried (MgSO4) and concentrated in vacuo. 6.4 g of pure product (73%) as colourless crystals was obtained by recrystallisation from ether/petroleum ether.
WORKUP
后处理
- custom(50° C./1013 mbar)
- filtrationThe mixture was then filtered
- concentrationconcentrated in vacuo
- additionCH2Cl2 (250 ml), NaHCO3 (100 ml) and water (300 ml) were added
- extractionThe organic layer was extracted with CHCl3
- dry with materialthis was dried (MgSO4)
- concentrationconcentrated in vacuo