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Methyl Acrylate → HCID 21079442, 화합물

HRID 1375105
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HRID 1375105 반응식
[CH3:1][CH:2]([CH3:11])[C:3](=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[C:12]([O:16][CH3:17])(=[O:15])[CH:13]=[CH2:14]>C1CCN2C(=NCCC2)CC1.C1CCCCC1>[CH3:17][O:16][C:12](=[O:15])[CH2:13][CH2:14][C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])([C:3](=[O:10])[CH:2]([CH3:1])[CH3:11])[CH2:3][CH2:4][C:5]([O:7][CH3:8])=[O:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 7294Methyl AcrylateHCID 81583Ethyl isobutyrylacetate

생성물 1

HCID 21079442HCID 21079442, 화합물수율 112.5%

시약·촉매·용매 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene촉매HCID 8078Cyclohexane용매

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온도
60 °C

실험 절차

12.0 g (0.08 mol) of ethyl 4-methyl-3-oxo-pentanoate and 0.5 g (0.003 mol) of DBU were placed in a three necked round bottom flask, equipped-with dropping funnel and reflux condenser. At room temperature, 16.0 g (0.18 mol) of methyl acrylate was slowly added drop by drop. After the exothermal behavior of the reaction leveled off, the reaction mixture was stirred at 60° C. for an additional two hours. The mixture was poured into cyclohexane and was washed with diluted hydrochloric acid and was subsequently washed with distilled water until the aqueous layer was neutral. The organic layer was dried over sodium sulfate, the solvent was removed, and the addition product was isolated by fractional distillation in a vacuum. 15.0 g (0.045 mol) of 4-(ethoxycarbonyl)-4-(2-methyl-1-oxopropyl)-heptanedioic acid 1,7-dimethyl ester was obtained (yield: 56%; boiling point: 145° C. at 0.02 mbar; colorless).

후처리

  1. temperaturereflux condenser
  2. customAt room temperature
  3. washwas washed with diluted hydrochloric acid
  4. washwas subsequently washed with distilled water until the aqueous layer
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe solvent was removed
  7. customthe addition product was isolated by fractional distillation in a vacuum

출처 및 근거

ORD 기록
ord-48f4518df1404a2dae24378b0559ee6a
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166648B2

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