反应详情

4-(2-Methoxy-ethyl)-2-oxo-piperidine-1,4-dicarboxylic acid 1-tert-butyl ester 4-ethyl ester (8.7 g) dissolved in dichloromethane (300 ml) under an argon atmosphere was treated with trifluoroacetic acid (60.32 g, 39.11 ml) and stirred for 3 hours at RT. The reaction mixture was then concentrated in vacuo, the residue dissolved in AcOEt, which was then washed with 3M aqueous NaOH, brine and dried over magnesium sulphate. The solvent was removed in vacuo and the residue was chromatographed on silica gel (acetone/CH2Cl2, gradient 0 to 10%) to give the desired product as light brown viscous oil (1.49 g). MS (ESI): 230.13 (MH+).

1. concentrationThe reaction mixture was then concentrated in vacuo
2. dissolutionthe residue dissolved in AcOEt
3. washwhich was then washed with 3M aqueous NaOH, brine
4. dry with materialdried over magnesium sulphate
5. customThe solvent was removed in vacuo
6. customthe residue was chromatographed on silica gel (acetone/CH2Cl2, gradient 0 to 10%)