反応 #56322

ord-0eabac01f602400795b8517efba6e5fe

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他equipped with a mechanical stirrer
  2. 2
    温度thermometer and reflux condenser
  3. 3
    ろ過After this time the reaction mixture was filtered
  4. 4
    workup.ADDITIONadditional sodium carbonate (5.0 grams) was added to the filtrate
  5. 5
    workup.DISTILLATIONvacuum distilled
  6. 6
    その他the fraction boiling at 123° C. and 0.05 mm of Hg pressure was collected

実験手順

2-n-Butoxyaniline (99 grams; 0.6 moles) and sodium carbonate (31.6 grams) were charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. 2-Bromomethyl-4,5-dimethyl-1,3-dioxolane (25 ml) was added and the reaction mixture was heated at a temperature of about 100° C. for a period of about 4 hours. After this time the reaction mixture was filtered and additional sodium carbonate (5.0 grams) was added to the filtrate. The mixture was then vacuum distilled and the fraction boiling at 123° C. and 0.05 mm of Hg pressure was collected to yield the desired product N-(4,5-dimethyl-1,3-dioxolan-2-ylmethyl)-2-n-butoxyaniline.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04225335uspto-grants-1980_09