Lithium Hydroxide → Deca-8-yl methacrylate

HRID 1460853

반응식

HRID 1460853 반응식
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]([OH:11])[CH2:9][CH3:10].[C:12](OC)(=[O:16])[C:13]([CH3:15])=[CH2:14].COC1C=CC(O)=CC=1.[OH-].[Li+]>O>[C:12]([O:11][CH:8]([CH2:9][CH3:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])(=[O:16])[C:13]([CH3:15])=[CH2:14]

참가 물질

6

반응물 4

HCID 3939Lithium HydroxideHCID 6658Methyl Methacrylate2회HCID 90154-MethoxyphenolHCID 5191583-Decanol

생성물 1

HCID 22140531Deca-8-yl methacrylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In the same reactor as used in Example 1, 760 kg (5 kmoles) of tricyclo[5.2.1.02,6 ]deca-8-yl alcohol and 1500 kg (15 kmoles) of methyl methacrylate were placed and well mixed with stirring. The water content of the mixture was 2500 ppm. To the mixture, 550 g of hydroquinone monomethyl ether and 3 kg of anhydrous lithium hydroxide were added to carry out the reaction. While refluxing methyl methacrylate through the distillation column, by-produced methanol was removed by distillation. The reaction was continued until almost no methanol was produced (about 7 hours). After removing unreacted methyl methacrylate by distillation under reduced pressure, the reaction mixture was cooled and filtered under pressure (2 kg/cm2) using a filter paper (pore size 0.1 mm, area 5 m2) placing thereon 10 kg of diatomaceous earth to yield 975 kg of tricyclo[5.2.1.02,6 ]deca-8-yl methacrylate with the filtrating time of 5.5 hours.

후처리

  1. additionwell mixed
  2. customthe reaction
  3. distillationthrough the distillation column
  4. customby-produced methanol
  5. customwas removed by distillation
  6. customwas produced (about 7 hours)
  7. customAfter removing unreacted methyl methacrylate
  8. distillationby distillation under reduced pressure
  9. temperaturethe reaction mixture was cooled
  10. filtrationfiltered under pressure (2 kg/cm2)

출처 및 근거

ORD 기록
ord-36f91bbf62784f6cb03d04cb620b72df
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05072027

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