反応 #2934

ord-ee33145d3712452584d543409e62c64a

反応方程式

C[Si](C)(C)OCCNCCO[Si](C)(C)C
bis(2-trimethylsilyloxylethyl)amine
CCN(CC)CC
triethylamine
O=S(=O)(Cl)c1ccccc1
benzenesulfonyl chloride
C[Si](C)(C)OCCN(CCO[Si](C)(C)C)S(=O)(=O)c1ccccc1
title compound
収率 88.0%
C[Si](C)(C)OCCN(CCO[Si](C)(C)C)S(=O)(=O)c1ccccc1
N,N-bis(2-trimethylsilyloxyethyl)benzenesulfonamide
収率 88.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added at 0° C.
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    workup.STIRRINGstirred further for 2 hours
  4. 4
    ろ過The reaction mixture was filtered
  5. 5
    workup.STIRRINGstirred further for 2 hours
  6. 6
    ろ過The reaction mixture was filtered
  7. 7
    workup.DISTILLATIONthe filtrate was subjected to vacuum distillation

実験手順

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)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05730953uspto-grants-1998_03