반응 #218765

ord-f2e1fbe248db484b8c7d8ecf412b18b8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The system was flushed thoroughly with nitrogen
  2. 2
    workup.STIRRINGstirred for 10 min
  3. 3
    여과The precipitate was filtered
  4. 4
    세척washed with water (100 ml)
  5. 5
    기타dried

실험 절차

Isovanillin (5 gm, 0.033 mol) was dissolved in glacial acetic acid (30 ml). Anhydrous sodium acetate (5.4 gm) was added to the above solution followed by powdered iron (0.15 gm). The system was flushed thoroughly with nitrogen. A solution of bromine (5.79 gm, 0.0362 mol) in glacial acetic acid (10 ml) was added to the above stirred suspension at room temperature over a period of 15 min. The reaction mixture was stirred at room temperature for 45 min. The reaction mixture was poured into aqueous 2% sodium bisulfite (200 ml) and stirred for 10 min. The precipitate was filtered washed with water (100 ml), and dried to obtain 3.5 gm of 2-bromoisovanillin as white powder mp: (200-202° C.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07384962B2uspto-grants-2008_06