反応 #160656

ord-54ad0f5650114efdb234fddac1cb1f15

反応方程式

CCCCOc1ccc(CC(=O)NO)cc1
bufexamac
CCCCOc1ccc(CC(=O)NO)cc1
2a
CCCCOc1ccc(CC(=O)NO)cc1
Bufexamac
COCC(C)O
1-methoxy-2-propanol
CCOC(N)=O
urethane
CCCCOc1ccc(CC(=O)NO)cc1
bufexamac
CCCCOc1ccc(CC(=O)NO)cc1
2a
CCCCOc1ccc(CC(=O)NO)cc1
Bufexamac
C=C(C)C(=O)[O-]
2b
C=C(C)C(=O)[O-]
Methacrylate
CC=Cc1ccccc1
Methylstyrene

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他respectively, were prepared
  2. 2
    その他The solution was then dried down to a powder, under vacuum, at 70° C
  3. 3
    その他A total of 4.93 grams of zirconia nanoparticle powder was recovered
  4. 4
    workup.ADDITIONredispersed in 4.93 grams of ultra-pure THF
  5. 5
    その他to yield a clear, slightly yellow solution
  6. 6
    workup.ADDITIONTo this solution 0.48 grams of 3-isopropenyl-α,α-dimethylbenzyl isocyanine was added
  7. 7
    その他The vial was sealed
  8. 8
    workup.STIRRINGstirred for 12 hours at room temperature

実験手順

Functionalized zirconia nanoparticles in which 50%, 25%, and 25% of the surface sites reacted with bufexamac, 2a (Preparatory Example 1), and 2b (Preparatory Example 2), respectively, were prepared as follows. A clean vial was charged with 10 grams of ZrO2 sol (47.3% weight) followed by 20 grams of 1-methoxy-2-propanol. Then 0.739 grams (0.70 mmol/g ZrO2) of bufexamac, 0.383 grams (0.35 mmol/g ZrO2) of 2a and 0.243 grams (0.35 mmol/g ZrO2) 2b were added to the vial. The content of the vial was stirred for 2 hours. The solution was then dried down to a powder, under vacuum, at 70° C. A total of 4.93 grams of zirconia nanoparticle powder was recovered. The powder was placed in a clean vial and redispersed in 4.93 grams of ultra-pure THF to yield a clear, slightly yellow solution. To this solution 0.48 grams of 3-isopropenyl-α,α-dimethylbenzyl isocyanine was added. The vial was sealed and stirred for 12 hours at room temperature. An FT-IR was taken of the sample, and an IR peak was observed at 1751 cm−1 and attributed to the ν(C═O) stretch in the urethane.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08829079B2uspto-grants-2014_09