反応 #577255

ord-a27161bfcc3e41a8b3f81e5b2f27f349

反応方程式

CCOc1cc(NC(C)=O)ccc1C(=O)NCC1CN(C(C)=O)CCO1
19
CCOc1cc(NC(C)=O)ccc1C(=O)NCC1CN(C(C)=O)CCO1
4-acetamido-N-((4-acetylmorpholin-2-yl)methyl)-2-ethoxybenzamide
O=C1CCC(=O)N1Cl
N-chlorosuccinimide
CCOc1cc(NC(C)=O)c(Cl)cc1C(=O)NCC1CN(C(C)=O)CCO1
20
収率 67.4%
CCOc1cc(NC(C)=O)c(Cl)cc1C(=O)NCC1CN(C(C)=O)CCO1
4-acetamido-N-((4-acetylmorpholin-2-yl)methyl)-5-chloro-2-ethoxybenzamide
収率 67.4%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction mixture was then concentrated under reduced pressure to dryness
  2. 2
    その他The residue was triturated with H2O
  3. 3
    その他the resulting solids were removed by filtration
  4. 4
    その他recrystallized from CH3OH

実験手順

A solution of 19 (1.78 g, 4.9 mmol) and N-chlorosuccinimide (0.687 g, 5.1 mmol, 1.05 equiv) in DMF (30 mL) was stirred for 1 h at 70° C. The reaction mixture was then concentrated under reduced pressure to dryness. The residue was triturated with H2O and the resulting solids were removed by filtration and recrystallized from CH3OH to yield 20 (1.314 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07528131B2uspto-grants-2009_05