HRID898748

反应详情

EQUATION

反应方程式

HRID 898748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butylamine (0.47 L, 6.4 mol) in THF (0.55 L) is slowly added, at 0° C., a solution of 4-nitrobenzenesulfonyl chloride (50 g, 0.23 mol) in THF (0.55 L) and the resulting mixture is stirred for 24 h at room temperature. The solvent is removed and the residue is taken up in a CHCl3/0.5 N HCl mixture, the layers are separated and the aqueous phase is extracted with CHCl3. The combined organic extracts are washed with H2O and brine and dried over MgSO4. The solvent is removed, yielding 56.3 g of a yellowish solid which is directly used in the next reaction (yield: 97%).

WORKUP

后处理

  1. customThe solvent is removed
  2. customthe layers are separated
  3. extractionthe aqueous phase is extracted with CHCl3
  4. washThe combined organic extracts are washed with H2O and brine
  5. dry with materialdried over MgSO4
  6. customThe solvent is removed