HRID2194000

反应详情

EQUATION

反应方程式

HRID 2194000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-(2-Methoxy-ethyl)-piperidine-4-carboxylic acid ethyl ester (0.646 g) dissolved in methylene chloride (10 ml) under an argon atmosphere were treated with DMAP (0.673 g) at RT, the mixture was cooled to 0° C. and morpholine-4-sulfonylchloride (0613 g) in methylene chloride (2 ml) was added dropwise. The mixture was stirred for 12 h at RT then partitioned between methylen chloride and 1 M HCl. The layers were separated, the organic layer washed with 2M aqueous KHCO3 then dried over Na2SO4. The solvent was evaporated off, the residue purified by flash chromatography (AcOEt/heptane, gradient from 0 to 50%) to give 4-(2-methoxy-ethyl)-1-(morpholine-4-sulfonyl)-piperidine-4-carboxylic acid ethyl ester, (0.68 g) as a light yellow solid. MS (ESI): 365.17 (MH+).

WORKUP

后处理

  1. customthen partitioned between methylen chloride and 1 M HCl
  2. customThe layers were separated
  3. washthe organic layer washed with 2M aqueous KHCO3
  4. dry with materialthen dried over Na2SO4
  5. customThe solvent was evaporated off
  6. customthe residue purified by flash chromatography (AcOEt/heptane, gradient from 0 to 50%)