反応 #1106661

ord-77bd4faca56641d7918889d62309813e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    その他The resulting solution was purged by nitrogen for 30 minutes before it
  3. 3
    その他to 72° C.
  4. 4
    その他for 18 hours
  5. 5
    workup.ADDITIONadded drop-wise into 400 mL of de-ionized water
  6. 6
    ろ過The solid was filtered with a frit funnel
  7. 7
    洗浄washed with water (2×200 ml)
  8. 8
    その他dried in a vacuum oven at 50° C. for 24 hours
  9. 9
    その他to afford 3.1 gram of P1 as white solid

実験手順

To a mixture of methacrylic acid (0.775 g, 9 mmol), 3-hydroxy-1 adamantylmethacrylate (1.42 g, 6 mmol), 9-anthrylmethylmethacrylate (1.38 g, 5 mmol) in 20 mL of tetrahydrofuran (THF) was added 2,2′-azobis(2-methylpropionitrile (0.16 g, 1 mmol). The resulting solution was purged by nitrogen for 30 minutes before it was heats to 72° C. for 18 hours under nitrogen. The solution was then cooled to room temperature and added drop-wise into 400 mL of de-ionized water. The solid was filtered with a frit funnel, washed with water (2×200 ml) and dried in a vacuum oven at 50° C. for 24 hours to afford 3.1 gram of P1 as white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08715907B2uspto-grants-2014_05