HRID265861

反应详情

EQUATION

反应方程式

HRID 265861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(N-Boc-4-piperidinyl)ethyl-amine (1-6) (0.45 g, 2.0 mmoles) in CHCl3 (20 ml) was treated with added triethylamine (0.405 g, 4.0 mmoles) followed by 3-chlorosulfonylbenzoyl chloride (3-1) (0.44 g, 2.0 mmoles) and the resulting solution was stirred at room temperature for 16 hours. The solvent was then removed and the residue was taken up in EtOAc and washed with H2O, 10% KHSO4 solution, brine and dried (Na2SO4). Solvent removal provided a residue that was purified by flash chromatography on silica gel eluting with CHCl3 (95)/MeOH(5) to give pure 4-1.

WORKUP

后处理

  1. customThe solvent was then removed
  2. washwashed with H2O, 10% KHSO4 solution, brine
  3. dry with materialdried (Na2SO4)
  4. customSolvent removal
  5. customprovided a residue that
  6. customwas purified by flash chromatography on silica gel eluting with CHCl3 (95)/MeOH(5)
  7. customto give pure 4-1