HRID1654102

反应详情

EQUATION

反应方程式

HRID 1654102 的结构方程式

PROCEDURE

实验过程

Ethyl bromoacetate (21.2 g, 0.127 mol) was added dropwise to a solution of 3-methoxycarbonylpiperidine (40 g, 0.254 mol) in diethyl ether (250 ml) at 0° C. The reaction was heated under reflux for 1 hour and the resulting precipitate filtered off and washed with diethyl ether. The ethereal solution was concentrated under reduced pressure to give the title compound (27.6 g); δ (60 MHz, CDCl3) 1.25 and 1.27 (each 3H, each t, J=7 Hz, 2×OCH2CH3). 1.40-3.70 (9H, m, 2CH2, 3CH, 4CH2, 5CH2 and 6CH2), 3.20 (2H, s, NCH2CO2), 4.10 and 4.15 (each 2H, each q, J=7 Hz, 2×NCH2CO2).

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureunder reflux for 1 hour
  3. filtrationthe resulting precipitate filtered off
  4. washwashed with diethyl ether
  5. concentrationThe ethereal solution was concentrated under reduced pressure