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Acetone → 1-[2-[(2-Methyl-1-oxo-2-propen-1-yl)oxy]ethyl] 1,2-cyclohexanedicarboxylate

HRID 1793278
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HRID 1793278 반응식
C[C:2]([CH3:4])=[O:3].[C@@H:5]12[C:14](=[O:15])[O:13][C:11](=[O:12])[C@@H:6]1[CH2:7][CH2:8][CH2:9][CH2:10]2.[C:16]([OH:21])(=[O:20])[C:17]([CH3:19])=[CH2:18]>O>[C:16]([O:21][CH2:4][CH2:2][O:3][C:11]([CH:6]1[CH2:7][CH2:8][CH2:9][CH2:10][CH:5]1[C:14]([OH:13])=[O:15])=[O:12])(=[O:20])[C:17]([CH3:19])=[CH2:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 180AcetoneHCID 4093Methacrylic AcidHCID 641660Hexahydrophthalic anhydride, cis-

생성물 1

HCID 64523861-[2-[(2-Methyl-1-oxo-2-propen-1-yl)oxy]ethyl] 1,2-cyclohexanedicarboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into acetone (1,000 ml) were dissolved cis-1,2-cyclohexane dicarboxylic anhydride (308.3 g), methacrylic acid (2-hydroxyethyl) (273.3 g) and 4-(dimethylamine) pyridine (4.9 g), and heated for 5 hours under reflux. After acetone had been distilled off under reduced pressure, 1N hydrochloric acid (500 ml) and ethyl acetate (2,000 ml) were added thereto so that an extracting process was carried out. After the organic layer had been washed with saturated saline solution (500 ml) twice, to this was added magnesium sulfuric anhydride (100 g) and this was allowed to stand for 1 hour to be dehydrated. After magnesium sulfate had been filtered and separated, ethyl acetate was distilled off under reduced pressure so that a white solid matter was obtained. After having been ground, this was added to water (2,000 ml), and after having been stirred for 2 hours, this was filtered and dried to obtain a white solid matter (518.9 g) of 2-[2-(methacryloyloxy)ethoxycarbonyl]cyclohexane carboxylic acid.

후처리

  1. temperatureheated for 5 hours
  2. temperatureunder reflux
  3. distillationAfter acetone had been distilled off under reduced pressure, 1N hydrochloric acid (500 ml) and ethyl acetate (2,000 ml)
  4. additionwere added
  5. washAfter the organic layer had been washed with saturated saline solution (500 ml) twice
  6. additionto this was added magnesium sulfuric anhydride (100 g)
  7. filtrationAfter magnesium sulfate had been filtered
  8. customseparated
  9. distillationethyl acetate was distilled off under reduced pressure so that a white solid matter
  10. customwas obtained
  11. filtrationthis was filtered
  12. customdried

출처 및 근거

ORD 기록
ord-156955290ae845ef8c4c29c66f5866ca
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07081329B2

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