反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]2[CH:8]=[C:9]([CH3:12])[CH:10]=[CH:11][C:4]=2[CH:3]=1.[CH3:13][C:14]1[CH:19]=[CH:18][C:17]2[CH:20]=[CH:21][C:22]([CH3:24])=[CH:23][C:16]=2[CH:15]=1>>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]2[CH:8]=[C:9]([CH3:12])[CH:10]=[CH:11][C:4]=2[CH:3]=1.[CH3:13][C:14]1[CH:19]=[CH:18][C:17]2[CH:20]=[CH:21][C:22]([CH3:24])=[CH:23][C:16]=2[CH:15]=1参加物
実験手順
It has been know that 2,6-DMN and 2,7-DMN form a eutectic crystal at a ratio 2,6-DMN/2,7-DMN of 0.7. Accordingly, in order to increase the recovery rate of 2,6-DMN, in a conventional cooling crystallization step, the feedstock is cooled so that the ratio 2,6-DMN/2,7-DMN in a mother liquor becomes approximately 0.7, and the material containing crystals thus formed is separated and purified (for example, recrystallization such as a high pressure crystallization method or treatment using a solvent). However, it was found by the inventors of the present invention that even when the material containing crystals thus formed was condensed by an effective solid-liquid separation method such as press filtration so that 60 wt % or more of 2,6-DMN was contained in the solid phase component, approximately 10 wt % of 2,7-DMN was also contained therein, and hence, it was difficult to obtain a 2,6-DMN having a purity of 99% or more by performing separation/purification of the solid phase component described above. In addition, through intensive research by the inventors of the present invention on the method for manufacturing a high purity 2,6-DMN having a purity of 99% or more, it was found that a reduction of the content of the 2,7-DMN contained in the solid phase component is important before the separation/purification was performed.
出典と根拠
- ORDレコード
- ord-0229152e148a4e61adc3da7e5ed7c6d8
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06525235B2
関連ノート
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