HRID265861
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
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
- customThe solvent was then removed
- washwashed with H2O, 10% KHSO4 solution, brine
- dry with materialdried (Na2SO4)
- customSolvent removal
- customprovided a residue that
- customwas purified by flash chromatography on silica gel eluting with CHCl3 (95)/MeOH(5)
- customto give pure 4-1