1-Octanol → Tetraoctyl pyromellitate

HRID 405687

반응식

HRID 405687 반응식
[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]

참가 물질

5

반응물 2

HCID 9571-OctanolHCID 6961Pyromellitic Acid

생성물 1

HCID 21895707Tetraoctyl pyromellitate수율 209%

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 7237O-Xylene용매

반응 조건

온도
160 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0c7ffbe529c247c1ac5f07b5d68037c1
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754019B2

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