反応 #40781

ord-bb9528bd65444948971ae1d9ea7916a5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONAdded
  2. 2
    温度The mixture was refluxed overnight
  3. 3
    濃縮Concentration
  4. 4
    その他on silica and purification with flash column chromatography (eluents PA:ether=95:5)

実験手順

Bis-(2-chloro-ethyl)-amine hydrochloride was suspended in 150 mL acetonitrile. Added were 34.8 g K2CO3 (3 equiv.) and 10.0 mL benzylbromide (1 equiv.). The mixture was refluxed overnight, Concentration on silica and purification with flash column chromatography (eluents PA:ether=95:5) yielded 4.11 g of a colorless oil. 1H NMR (400 MHz, CDCl3) δ 2.93 (t, J=7 Hz, 4H), 3.50 (t, J=7 Hz, 4H), 3.74 (s, 2H), 7.22-7.37 (m, 5H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07728018B2uspto-grants-2010_06