Sulfuric Acid → Glyceryl methacrylate

HRID 1438689

반응식

HRID 1438689 반응식
[C:1]([O:6][CH2:7][CH:8]1[O:10][CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].S(=O)(=O)(O)[OH:12].[OH-].[Na+]>O>[C:1]([O:6][CH2:7][CH:8]([CH2:9][OH:12])[OH:10])(=[O:5])[C:2]([CH3:4])=[CH2:3]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 7837Glycidyl methacrylateHCID 14798Sodium Hydroxide

생성물 1

HCID 65442Glyceryl methacrylate수율 2.19%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Two hundred grams (1.406 mole) of glycidyl methacrylate, 300 ml of water and 0.5 ml of concentrated sulfuric acid are stirred for 5 days at 24-29° C. A clear solution forms having a pH of 2.0 which is neutralized with 10% sodium hydroxide. The solution is extracted with six 100 ml portions of ethyl ether. The aqueous layer is stirred and saturated with sodium sulfate which is then extracted with six 100 ml portions of methylene chloride. The methylene chloride extracts are concentrated under reduced pressure to yield 118.7 grams of glyceryl methacrylate containing 2.19% unreacted glycidyl methacrylate. 62.6 gm of this material is mixed with 26.1 gm of methyl methacrylate. The mixture is combined with 18.2 mg of isopropyl percarbonate, and separated into four test tubes. Nitrogen is bubbled through each tube, the tubes arecooled to - 30° C, evacuated, filled with nitrogen, sealed under vacuum, and put into a constant temperature bath at 40° C for 5 hours. The tubes are then put in an oven held at 75° C overnight. The next morning, the temperature is increased to 90° C for one hour. The tubes are then cooled and broken to provide a solid rod of polymer.

후처리

  1. extractionThe solution is extracted with six 100 ml portions of ethyl ether
  2. extractionis then extracted with six 100 ml portions of methylene chloride
  3. concentrationThe methylene chloride extracts are concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-194e5f484c4344a790270e2d535eae2a
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04056496

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