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Diethyl Oxalate → HCID 15870414, 화합물

HRID 379687
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HRID 379687 반응식
[Na].[C:2]([O:9][CH2:10][CH3:11])(=[O:8])[C:3]([O:5]CC)=O.[CH3:12][C:13]1[CH:18]=[C:17]([CH3:19])[CH:16]=[C:15]([CH3:20])[C:14]=1[C:21](=[O:25])[CH2:22][CH2:23][CH3:24]>CCO>[CH2:23]([CH:22]([C:21](=[O:25])[C:14]1[C:15]([CH3:20])=[CH:16][C:17]([CH3:19])=[CH:18][C:13]=1[CH3:12])[C:3](=[O:5])[C:2]([O:9][CH2:10][CH3:11])=[O:8])[CH3:24]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7268Diethyl OxalateHCID 2511601-(2,4,6-Trimethylphenyl)butan-1-oneHCID 5360545Sodium2회

생성물 1

HCID 15870414HCID 15870414, 화합물수율 53.2%

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
50 °C

실험 절차

Sodium (1.0 g, 42.1 mmol, spheres was cautiously added to 25 mL of absolute EtOH with stirring. After the sodium had dissolved, diethyl oxalate (6.0 g, 42.1 mmol) was added dropwise to the resulting solution at 0° C., followed by addition of a solution of 2′,4′,6′-trimethylbutyrophenone (8 g, 42.1 mmol) in 5 mL of absolute EtOH. The reaction zmixture was slowly warmed to 50° C. and stirred overnight. The solvent was then evaporated. The resulting residue was washed with hexane, diluted with water, acidified with 1 N HCl, and then extracted with ether. The extracts were washed with brine, dried over Na2SO4 and concentrated to give 6.5 g of an oil which was used in the next reaction without farther purification.

후처리

  1. stirringstirred overnight
  2. customThe solvent was then evaporated
  3. washThe resulting residue was washed with hexane
  4. additiondiluted with water
  5. extractionextracted with ether
  6. washThe extracts were washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-70311de3fa71442e940a26947180f5bf
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06300360B1

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