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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → 4'-Pentyl-bicyclohexyl-4-carboxylic acid 3-(2-methyl-acryloyloxy)-propyl ester

HRID 386326
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HRID 386326 반응식
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[H-].[Na+].Br[CH2:10][CH2:11][CH2:12][O:13][C:14]([CH:16]1[CH2:21][CH2:20][CH:19]([CH:22]2[CH2:27][CH2:26][CH:25]([CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:24][CH2:23]2)[CH2:18][CH2:17]1)=[O:15].O>CN(C)C=O>[CH3:3][C:2](=[CH2:4])[C:1]([O:6][CH2:10][CH2:11][CH2:12][O:13][C:14]([CH:16]1[CH2:21][CH2:20][CH:19]([CH:22]2[CH2:23][CH2:24][CH:25]([CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:26][CH2:27]2)[CH2:18][CH2:17]1)=[O:15])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 4093Methacrylic AcidHCID 24758Sodium hydrideHCID 59289083HCID 59289083, 화합물

생성물 1

HCID 592890824'-Pentyl-bicyclohexyl-4-carboxylic acid 3-(2-methyl-acryloyloxy)-propyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

A solution of methacrylic acid (3.5 g, 40.7 mmol) in dimethylformamide (100 ml) is added dropwise to an ice cooled slurry of sodium hydride (60% suspension in paraffin oil) (1.6 g, 40.0 mmol) in dimethylformamide (100 ml). Once addition is complete, the mixture is allowed to warm to room temperature and is stirred for 1 h, the intermediate 4′-pentyl-bicyclohexyl-4-carboxylic acid 3-bromo-propyl ester (15.0 g, 37.4 mmol) in dimethylformamide (100 ml) is added dropwise. The mixture is stirred at 50° C. overnight. The mixture is cooled to room temperature, poured into icy water, and this is extracted three times with DCM. The DCM solution is washed with brine, water and then dried over sodium sulphate. The solution is evaporated to dryness and recrystallised from industrial methylated spirits to afford a white crystalline solid.

후처리

  1. additionOnce addition
  2. stirringThe mixture is stirred at 50° C. overnight
  3. temperatureThe mixture is cooled to room temperature
  4. extractionthis is extracted three times with DCM
  5. washThe DCM solution is washed with brine, water
  6. dry with materialdried over sodium sulphate
  7. customThe solution is evaporated to dryness
  8. customrecrystallised from industrial methylated spirits
  9. customto afford a white crystalline solid

출처 및 근거

ORD 기록
ord-88a368d43ae244c6a3c511f9e519d674
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372307B2

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