반응 #2374825

ord-8ec299064ffe4d189fd8025df6cff4e3

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was then refluxed in a nitrogen stream for 10 hours
  2. 2
    기타After the completion of the reaction
  3. 3
    기타Yellow crystals precipitated at this point
  4. 4
    기타were separated through filtration
  5. 5
    기타recrystallized from chloroform

실험 절차

Ten grams (30.9 mmols) of crude 2-(3'-N,N-diethylaminomethyl-2'-hydroxy-5'-methylphenyl)-2H-benzotriazole obtained following the procedures of Synthesis Example 1 and 10.5 g (31.1 mmols) of 2-(2'-hydroxy-5'-methacryloyloxypropylphenyl)-2H-benzotriazole were dissolved in 64 ml of xylene, and 1.5 ml of a 28% sodium methylate-methanol solution were added thereto. The mixture was then refluxed in a nitrogen stream for 10 hours. After the completion of the reaction, the reaction mixture was cooled to room temperature. Yellow crystals precipitated at this point were separated through filtration, and recrystallized from chloroform to obtain 12.8 g of 6-(2H-benzotriazol-2-yl)-4-methacryloyloxypropyl-2-[3'-(2H-benzotriazol-2-yl)-2'-hydroxy-5'-methylphenyl]methylphenol (hereinafter abbreviated as "RUVA-3") as white crystals (yield 71.0%, purity 98.6%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06084104uspto-grants-2000_07