반응 #56323

ord-e99f9d76b08a481ba3c31cb20e20a62f

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타equipped with a mechanical stirrer
  2. 2
    온도thermometer and reflux condenser
  3. 3
    여과After 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
    기타the fraction boiling at 120° C. and 0.07 mm of Hg pressure was collected

실험 절차

2-Methoxyaniline (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-methyl-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 120° C. and 0.07 mm of Hg pressure was collected to yield the desired product N-(4-methyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04225335uspto-grants-1980_09