反応 #56595

ord-92f36e32dd5d4bacbd6092f3ab38af0a

反応方程式

CN(C)c1ccc(N=Nc2ccc(N=Nc3ccc(O)c4ccccc34)cc2)c2ccccc12
1-[4-(4-(dimethylamino)naphthylazo)phenylazo]-4-hydroxy-naphtalene
C=CC(=O)OCCCCCCI
6-iodohexyl acrylate
O=C([O-])[O-].[K+].[K+]
potassium carbonate
C=CC(=O)OCCCCCCOc1ccc(N=Nc2ccc(N=Nc3ccc(N(C)C)c4ccccc34)cc2)c2ccccc12
1-[4-(4-(dimethylamino)naphthylazo)-phenylazo]-4-(6-acryloyloxyhexyloxy)naphtalene
収率 84.4%

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling to room temperature the reaction mixture
  2. 2
    その他was quenched with 100 ml 3N HCl
  3. 3
    ろ過the resulting precipitate was filtered off
  4. 4
    洗浄washed with water (100 ml) and ethanol (50 ml)

実験手順

A mixture consisting of 0.44 g of 1-[4-(4-(dimethylamino)naphthylazo)phenylazo]-4-hydroxy-naphtalene, 0.56 g of 6-iodohexyl acrylate, and 0.28 g of potassium carbonate in 10 ml of DMF was stirred under nitrogen atmosphere for 3 h at 60° C. After cooling to room temperature the reaction mixture was quenched with 100 ml 3N HCl and the resulting precipitate was filtered off, washed with water (100 ml) and ethanol (50 ml) to give 0.5 g of pure 1-[4-(4-(dimethylamino)naphthylazo)-phenylazo]-4-(6-acryloyloxyhexyloxy)naphtalene as a brownish powder; λmax. (CB 483): 504 nm.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07419620B2uspto-grants-2008_09