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Potassium Hydroxide → 944142-61-4

HRID 1777350
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HRID 1777350 반응식
[OH-].[K+].[OH-].[Na+].C([O:7][C:8]([C:10]1([CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1)=[O:9])C>O.C(O)C>[C:19]([O:18][C:16]([N:13]1[CH2:14][CH2:15][C:10]([CH2:23][CH:24]([CH3:26])[CH3:25])([C:8]([OH:9])=[O:7])[CH2:11][CH2:12]1)=[O:17])([CH3:22])([CH3:21])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 14798Sodium HydroxideHCID 59327423HCID 59327423, 화합물

생성물 1

HCID 57790581944142-61-4

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of potassium hydroxide (85% assay, 2.69 g, 0.041 mol) and sodium hydroxide (1.94 g, 0.048 mol) in demineralized water (8 mL) is added to a solution of 4-isobutylpiperidine-1,4-dicarboxylic acid-1-tertbutyl ester-4-ethyl ester (0.95 g, 0.003 mol) in ethanol (15 mL). The reaction mixture is refluxed for 48 hrs. It is cooled to room temperature, concentrated under reduced pressure, and then treated with demineralized water (10 mL). The pH is adjusted to ˜3-4 using 2N HCl (10 mL) and the aqueous layer is extracted with ethyl acetate (2×15 mL). The combined extract is dried over sodium sulfate. Removal of solvent gives a crude residue which is purified by column chromatography (230-400 mesh, ethyl acetate:n-hexane 1:3) to furnish 4-isobutylpiperidine-1,4-dicarboxylic acid monotertbutyl ester.

후처리

  1. temperatureThe reaction mixture is refluxed for 48 hrs
  2. concentrationconcentrated under reduced pressure
  3. additiontreated with demineralized water (10 mL)
  4. extractionthe aqueous layer is extracted with ethyl acetate (2×15 mL)
  5. extractionThe combined extract
  6. dry with materialis dried over sodium sulfate
  7. customRemoval of solvent
  8. customgives a crude residue which
  9. customis purified by column chromatography (230-400 mesh, ethyl acetate:n-hexane 1:3)

출처 및 근거

ORD 기록
ord-035931fb71b1432eb8d34774d5764556
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266867B2

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