反応 #56312

ord-b450100da9fe427db4334b43432f4259

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 (5.00 grams) was added to the filtrate
  5. 5
    workup.DISTILLATIONThe mixture was then distilled under reduced pressure

実験手順

2-Methoxyaniline (87 ml; 0.7 mole) and sodium carbonate (31.66 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 mls) was added and the reaction mixture was heated at a temperature of 100° C. for a period of about 4 hours. After this time the reaction mixture was filtered and additional sodium carbonate (5.00 grams) was added to the filtrate. The mixture was then distilled under reduced pressure to yield the desired product N-(4,5-dimethyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline boiling at 125° to 128° C. at 0.1 mm of Hg pressure.

出典

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