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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → 4'-Propyl-bicyclohexyl-4-carboxylic acid 3-acryloyloxy-propyl ester

HRID 386327
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인쇄 미리보기

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HRID 386327 반응식
[C:1]([O-:5])(=[O:4])[CH:2]=[CH2:3].[Na+].CC(=C)C(OCCC[CH2:15][CH2:16][CH2:17][O:18][C:19]([CH:21]1[CH2:26][CH2:25][CH:24]([CH:27]2[CH2:32][CH2:31][CH:30]([CH2:33][CH2:34][CH2:35]CC)[CH2:29][CH2:28]2)[CH2:23][CH2:22]1)=[O:20])=O.[I-].[Na+].O>CN(C)C=O>[C:1]([O:5][CH2:15][CH2:16][CH2:17][O:18][C:19]([CH:21]1[CH2:26][CH2:25][CH:24]([CH:27]2[CH2:28][CH2:29][CH:30]([CH2:33][CH2:34][CH3:35])[CH2:31][CH2:32]2)[CH2:23][CH2:22]1)=[O:20])(=[O:4])[CH:2]=[CH2:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 5238Sodium IodideHCID 4068533Sodium acrylateHCID 592890404'-Pentyl-bicyclohexyl-4-carboxylic acid 6-(2-methyl-acryloyloxy)-hexyl ester

생성물 1

HCID 592890704'-Propyl-bicyclohexyl-4-carboxylic acid 3-acryloyloxy-propyl ester

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

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온도
130 °C

실험 절차

A mixture of sodium acrylate (2.5 g, 13.4 mmol), 4′-propyl-bicyclohexyl-4-carboxylic acid 3-bromo-propyl ester (synthesis described for preferred example 1) (5.0 g, 13.4 mmol) and sodium iodide (2.5 g, 16.7 mmol) in dimethylformamide (150 ml) is stirred at 130° C. overnight. The mixture is cooled to room temperature, poured into water, and this is extracted twice with diethyl ether. The ethereal solution is washed with water and then dried over sodium sulphate. The solution is evaporated to dryness and purified by flash column chromatography using DCM/petrol (1/1) as eluant to give upon evaporation of the appropriate fractions a colourless oil.

후처리

  1. temperatureThe mixture is cooled to room temperature
  2. extractionthis is extracted twice with diethyl ether
  3. washThe ethereal solution is washed with water
  4. dry with materialdried over sodium sulphate
  5. customThe solution is evaporated to dryness
  6. custompurified by flash column chromatography
  7. customto give upon evaporation of the appropriate fractions a colourless oil

출처 및 근거

ORD 기록
ord-3352ca3e5f3a43e796f555dd60c1a09a
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372307B2

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