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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethanol → Benzenebutanenitrile, beta-oxo-alpha-(3-(trifluoromethyl)phenyl)-

HRID 1589093
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HRID 1589093 반응식
[Na].C(O)C.[F:5][C:6]([F:17])([F:16])[C:7]1[CH:8]=[C:9]([CH2:13][C:14]#[N:15])[CH:10]=[CH:11][CH:12]=1.[C:18]1([CH2:24][C:25](OCC)=[O:26])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>O>[F:5][C:6]([F:16])([F:17])[C:7]1[CH:8]=[C:9]([CH:13]([C:25]([CH2:24][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[O:26])[C:14]#[N:15])[CH:10]=[CH:11][CH:12]=1
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참가 물질

6

반응물 4

HCID 702EthanolHCID 7590Ethyl phenylacetateHCID 75360m-TrifluoromethylphenylacetonitrileHCID 5360545Sodium2회

생성물 1

HCID 106559Benzenebutanenitrile, beta-oxo-alpha-(3-(trifluoromethyl)phenyl)-수율 73.5%

시약·촉매·용매 1

HCID 962Water
용매

실험 절차

In this example, 4.91 g of metallic sodium was added to 110 ml of anhydrous ethanol at room temperature and stirred until all of the sodium dissolved. A mixture containing 18.76 g of (3-trifluoromethylphenyl)acetonitrile and 21.73 g of ethyl phenylacetate was then added dropwise and the resulting mixture was stirred at reflux for about 18 hours. The mixture was then poured into 300 ml water and extracted three times with ethyl ether. The pH of the extracted aqueous layer was adjusted to a pH of about 1 with aqueous 10 wt. % hydrochloric acid and again extracted three times with ethyl ether. The organic layer was washed twice with saturated aqueous sodium bicarbonate, dried over magnesium sulfate and evaporated to dryness under vacuum affording 22.6 g of the title compound.

후처리

  1. dissolutiondissolved
  2. additionwas then added dropwise
  3. temperatureat reflux for about 18 hours
  4. extractionextracted three times with ethyl ether
  5. extractionagain extracted three times with ethyl ether
  6. washThe organic layer was washed twice with saturated aqueous sodium bicarbonate
  7. dry with materialdried over magnesium sulfate
  8. customevaporated to dryness under vacuum

출처 및 근거

ORD 기록
ord-49605d1b4eb54723b0e3d3e2e958f459
출처 데이터셋
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04568376

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