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
To a solution of 2-methyl-1-[3-(N-hexadecanoyl)aminopropyl]piperidine (0.47 g, 1.2 mmole) in diethyl ether was added an ethereal solution of hydrogen chloride. The reaction mixture was placed in the refrigerator overnight. The precipitate was filtered. The gummy paste was dissolved in methanol and the solvent removed under reduced pressure to give the title compound (0.37 g, 71%) as a pale paste. 1H NMR (300 MHz, CDCl3): mixture of rotamers, major peaks given. δ0.870 (H, t, J=6.7 Hz), 1.243 (24H, bs), 1.533 (3H, d, J=6.4 Hz), 1.59 to 1.66 (2H, m), 1.81 to 1.88 (2H, m), 2.06 to 2.70 (8H, m), 2.74 to 3.10 (2H, m), 3.12 to 3.70 (3H, m), and 7.264 (1H, bs). IR (neat): 2686, 1941, 1649, 1549, 1468, 1379, 1230, and 1123 cm-1. Analysis calculated for C25H51CIN2O.3/4H2O: C, 67.53; H, 11.90; N, 6.30; Cl, 7.97. Found: C, 67.55; H, 11.85; N, 6.29; Cl, 8.04.
WORKUP
后处理
- customwas placed in the refrigerator overnight
- filtrationThe precipitate was filtered
- dissolutionThe gummy paste was dissolved in methanol
- customthe solvent removed under reduced pressure