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Water → HCID 12115477, 화합물

HRID 2373328
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HRID 2373328 반응식
[H-].[Li+].[Al+3].[H-].[H-].[H-].[CH3:7][CH:8]([C:13]1[CH:19]=[C:18]([C:20](F)([C:25]([F:28])([F:27])[F:26])[C:21]([F:24])([F:23])[F:22])[CH:17]=[CH:16][C:14]=1[NH2:15])[CH2:9][CH:10]([CH3:12])[CH3:11].O.S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1>[CH3:7][CH:8]([C:13]1[CH:19]=[C:18]([CH:20]([C:21]([F:22])([F:23])[F:24])[C:25]([F:27])([F:28])[F:26])[CH:17]=[CH:16][C:14]=1[NH2:15])[CH2:9][CH:10]([CH3:11])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24083Sulfuric acid magnesium salt (1:1)HCID 21226445Aluminium lithium hydrideHCID 22734601HCID 22734601, 화합물

생성물 1

HCID 12115477HCID 12115477, 화합물수율 98.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

Aluminum lithium hydride (2 g, 52.7 mmol) was suspended in tetrahydrofuran (60 ml), followed by adding dropwise thereto 2-(1,3-dimethylbutyl)-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]aniline (14 g, 40.5 mmol), and the resulting mixture was stirred at reflux temperature for 3 hours. Water was added to the reaction mixture in small portions under ice-cooling, followed by stirring for 10 minutes. Magnesium sulfate was added thereto and then stirred for 10 minutes. The reaction mixture was filtered through Celite and the filtrate was concentrated under reduced pressure to obtain 13 g of the desired compound.

후처리

  1. additionby adding dropwise
  2. temperatureat reflux temperature for 3 hours
  3. temperaturecooling
  4. stirringstirred for 10 minutes
  5. filtrationThe reaction mixture was filtered through Celite
  6. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7d948fc099af47f392b2d1d997b3c77a
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07459477B2

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