Reaktion #1106661

ord-77bd4faca56641d7918889d62309813e

Reaktionsgleichung

CC(C)C#N
2-methylpropionitrile
C=C(C)C(=O)O
methacrylic acid
CC(=CC12CC3CC(CC(O)(C3)C1)C2)C(=O)[O-]
3-hydroxy-1 adamantylmethacrylate
C=C(C)C(=O)OCc1c2ccccc2cc2ccccc12
9-anthrylmethylmethacrylate
C=CC(=O)OC12CC3CC(CC(O)(C3)C1)C2
HADMA

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08715907B2uspto-grants-2014_05