1-Octanol → Tetraoctyl pyromellitate

HRID 405687

反応式

HRID 405687 の反応式
[C:1]([OH:18])(=[O:17])[C:2]1[C:3](=[CH:7][C:8](=[C:12]([CH:16]=1)[C:13]([OH:15])=[O:14])[C:9]([OH:11])=[O:10])[C:4]([OH:6])=[O:5].[CH2:19](O)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4].C1(C)C(C)=CC=CC=1>[C:9]([O:11][CH2:9][CH2:8][CH2:7][CH2:3][CH2:2][CH2:16][CH2:12][CH3:13])(=[O:10])[C:8]1[C:12](=[CH:16][C:2](=[C:3]([CH:7]=1)[C:4]([O:6][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:5])[C:1]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:17])[C:13]([O:15][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:14]

参加物

5

反応物 2

HCID 9571-OctanolHCID 6961Pyromellitic Acid

生成物 1

HCID 21895707Tetraoctyl pyromellitate収率 209%

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒HCID 7237O-Xylene溶媒

反応条件

温度
160 °C

実験手順

To a 2-liter four necked flask equipped with Dean Stark apparatus, 218 g of anhydrous pyromellitic acid, 650 g of n-octanol, 0.2 g of titanium tetraisopropoxide and 300 cc of xylene were added and reacted with stirring at 160 degrees C. for 4 hours under nitrogen stream while distilling water. Subsequently, washing by saturated brine and washing by 0.1 N aqueous sodium hydroxide were respectively conducted three times, followed by being dried by anhydrous magnesium sulfate. After magnesium sulfate was filtered, unreacted alcohol was distilled under reduced pressure to obtain 630 g of tetraoctyl pyromellitate. Tetraoctyl pyromellitate, regarded as Comparative Example 3, was similarly measured with respect to the properties.

後処理

  1. additionwere added
  2. customreacted
  3. distillationfor 4 hours under nitrogen stream while distilling water
  4. washSubsequently, washing by saturated brine
  5. washwashing by 0.1 N aqueous sodium hydroxide
  6. dry with materialby being dried by anhydrous magnesium sulfate
  7. filtrationAfter magnesium sulfate was filtered
  8. distillationunreacted alcohol was distilled under reduced pressure

出典と根拠

ORDレコード
ord-0c7ffbe529c247c1ac5f07b5d68037c1
出典データセット
uspto-grants-2014_06
特許番号
US08754019B2

関連ノート

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