反応 #73934

ord-0419d431c2244390b16ea63e4a4f739a

反応方程式

O=C(CBr)c1ccccc1
2-bromo-1-phenylethanone
CNCc1ccc(Cl)cc1Cl
(2,4-dichlorophenyl)-N-methylmethanamine
CCN(CC)CC
Triethylamine
CN(CC(=O)c1ccccc1)Cc1ccc(Cl)cc1Cl
title compound
収率 90.0%
CN(CC(=O)c1ccccc1)Cc1ccc(Cl)cc1Cl
2-((2,4-dichlorobenzyl)(methyl)amino)-1-phenylethanone
収率 90.0%

反応条件

温度
20°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Into a 50-mL 3-necked round-bottom flask purged
  2. 2
    温度maintained with an inert atmosphere of nitrogen
  3. 3
    workup.STIRRINGThe resulting solution was stirred for 1 h at 20° C. in an oil bath
  4. 4
    ろ過The solids were filtered out
  5. 5
    濃縮The resulting mixture was concentrated under vacuum

実験手順

Into a 50-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 2-bromo-1-phenylethanone (1 g, 5.05 mmol, 1.00 equiv) in 1,4-dioxane (20 mL) and (2,4-dichlorophenyl)-N-methylmethanamine (1.1 g, 5.82 mmol, 1.15 equiv). Triethylamine (2 g, 19.80 mmol, 3.92 equiv) was added dropwise with stirring at 20° C. The resulting solution was stirred for 1 h at 20° C. in an oil bath. The solids were filtered out. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:50). This resulted in 1.4 g (90%) of the title compound as a yellow oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541448B2uspto-grants-2013_09