Water → Deca-8-yl methacrylate

HRID 1460852

반응식

HRID 1460852 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].O.COC1C=CC(O)=CC=1>CO>[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 962WaterHCID 6658Methyl MethacrylateHCID 90154-MethoxyphenolHCID 5191583-Decanol

생성물 1

HCID 22140531Deca-8-yl methacrylate

시약·촉매·용매 1

HCID 887Methanol용매

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 kmole) of methyl methacrylate were placed and well mixed with stirring. The water content of the resulting mixture was 2500 ppm. To the mixture, 550 g of hydroquinone monomethyl ether was added and heated while introducing thereinto dried air at a rate of 4 m3/ hr and reluxing methyl methacrylate through the distillation column to remove water by azeotropic distillation. After 1 hour from the beginning of the reflux of methyl methacrylate, the water content in the reactor became 630 ppm. Then, 3 kg of anhydrous lithium hydroxide was charged into the reactor to carry out the reaction. While removing methanol by-produced by the reaction from the reaction system by distillation, the reaction was continued until almost no methanol was distilled (about 7 hours), followed by removal of unreacted methyl methacrylate under reduced pressure. After cooling, the mixture was 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 990 kg of tricyclo[5.2.1.02,6 ]deca-8-yl methacrylate with the filtrating time of 2 hours.

후처리

  1. additionwell mixed
  2. temperatureheated
  3. additionwhile introducing
  4. dry with materialthereinto dried air at a rate of 4 m3/ hr and reluxing methyl methacrylate
  5. distillationthrough the distillation column
  6. customto remove water
  7. distillationby azeotropic distillation
  8. temperatureAfter 1 hour from the beginning of the reflux of methyl methacrylate
  9. additionThen, 3 kg of anhydrous lithium hydroxide was charged into the reactor
  10. customthe reaction
  11. customWhile removing methanol
  12. customby-produced by the reaction from the reaction system by distillation
  13. distillationwas distilled (about 7 hours)
  14. customfollowed by removal of unreacted methyl methacrylate under reduced pressure
  15. temperatureAfter cooling
  16. filtrationthe mixture was filtered under pressure (2 kg/cm2)

출처 및 근거

ORD 기록
ord-2d7c1fd66c084b368b45f05645246858
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05072027

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