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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2,2,2,4'-Tetrafluoroacetophenone → 2,2,2-Trifluoro-1-(4-fluoro-phenyl)-1-[4-(1,1,1,3,3,3-hexamethyl disilazan-2-yl)-3,5-dimethyl-phenyl]-ethanol

HRID 1917052
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HRID 1917052 반응식
Br[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N:9]([Si:14]([CH3:17])([CH3:16])[CH3:15])[Si:10]([CH3:13])([CH3:12])[CH3:11])=[C:4]([CH3:18])[CH:3]=1.C([Li])CCC.[F:24][C:25]([F:36])([F:35])[C:26]([C:28]1[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=1)=[O:27]>O1CCCC1>[F:36][C:25]([F:24])([F:35])[C:26]([C:28]1[CH:29]=[CH:30][C:31]([F:34])=[CH:32][CH:33]=1)([C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N:9]([Si:14]([CH3:17])([CH3:16])[CH3:15])[Si:10]([CH3:13])([CH3:12])[CH3:11])=[C:4]([CH3:18])[CH:3]=1)[OH:27]
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HCID 695642,2,2,4'-TetrafluoroacetophenoneHCID 594978222-(4-Bromo-2,6-dimethyl-phenyl)-1,1,1,3,3,3-hexamethyl-disilazaneHCID 178418339Butyllithium

생성물 1

HCID 594978232,2,2-Trifluoro-1-(4-fluoro-phenyl)-1-[4-(1,1,1,3,3,3-hexamethyl disilazan-2-yl)-3,5-dimethyl-phenyl]-ethanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2-(4-bromo-2,6-dimethyl-phenyl)-1,1,1,3,3,3-hexamethyl-disilazane (Example II) (1.72 g, 5.0 mmol) in tetrahydrofuran (12 ml) under a nitrogen atmosphere was slowly added a solution of n-butyl lithium in hexanes (1.6 M) (3.3 ml, 5.28 mmol) at −70° C. The reaction mixture was stirred at −70° C. for 30 minutes before addition of 2,2,2,4′-tetrafluoroacetophenone (commercially available) (1.01 g, 5.25 mmol) at −70° C. The cooling bath was removed after 15 minutes. Once the reaction mixture had reached ambient temperature, it was poured onto water. The mixture was extracted with diethyl ether. The organic phase was washed with water and brine, dried over sodium sulfate, and then concentrated. The title compound was isolated as a yellow oil.

후처리

  1. customThe cooling bath was removed after 15 minutes
  2. customhad reached ambient temperature
  3. additionit was poured onto water
  4. extractionThe mixture was extracted with diethyl ether
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fd90c40e3b4d43f995710731cd943f44
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08618173B2

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