HRID2838

反应详情

EQUATION

反应方程式

HRID 2838 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 4.97 g of bis(2-trimethylsilyloxylethyl)amine, 3.03 g of triethylamine and 50 ml of benzene, 3.21 g of benzenesulfonyl chloride was added at 0° C. under stirring. After the addition, the mixture was taken out of the cooling bath and stirred further for 2 hours. The reaction mixture was filtered, mixture was taken out of the cooling bath and stirred further for 2 hours. The reaction mixture was filtered, and the filtrate was subjected to vacuum distillation. The residue was passed through a silica gel column with the eluent varying from benzene to benzen-acetic acid (9:1). As a result, 6.23 g of the title compound was obtained as a colorless oily substance. NMRδ: 7.83 (2H,d,J=8.0 Hz),7.52 (3H,m), 3.72, 3.31 (each 4H,t,J=6.5 Hz), 0.09 (18H,s)

WORKUP

后处理

  1. additionwas added at 0° C.
  2. additionAfter the addition
  3. stirringstirred further for 2 hours
  4. filtrationThe reaction mixture was filtered
  5. stirringstirred further for 2 hours
  6. filtrationThe reaction mixture was filtered
  7. distillationthe filtrate was subjected to vacuum distillation