反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of (±) cis-1-(3,4-dichlorobenzyl)-2-(N-methyl-N-tert-butoxycarbonyl-amino)indane (1.016 g, 2.5 mmol) in dichloromethane (20 ml) at 0° C. was added trifluoroacetic acid (4 ml) dropwise. The solution was then stirred at room temperature for 2 h, poured into saturated aqueous NaHCO3 (150 ml) and extracted with dichloromethane (3×30 ml). The combined organic phases were dried over sodium sulfate, and concentrated in vacuo. The residue was subjected to column chromatography on silica eluting with 5% ethanol in chloroform to afford the title compound as a colourless oil (585 mg) which was converted to the HCl salt and crystallised to afford a white solid. m.p.>245° C. dec. (from ethanol-diethyl ether).
WORKUP
后处理
- extractionextracted with dichloromethane (3×30 ml)
- dry with materialThe combined organic phases were dried over sodium sulfate
- concentrationconcentrated in vacuo