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Hydrochloric Acid → 1-(4-Bromo-1-naphthalenyl)-3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxy-1-butanone

HRID 1895404
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HRID 1895404 반응식
C([N-]C(C)C)(C)C.[Li+].[Br:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([C:20](=[O:22])[CH3:21])=[CH:12][CH:11]=1.[Cl:23][C:24]1[CH:25]=[C:26]([C:31](=[O:36])[C:32]([F:35])([F:34])[F:33])[CH:27]=[C:28]([Cl:30])[CH:29]=1.Cl>O1CCCC1>[Br:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([C:20](=[O:22])[CH2:21][C:31]([C:26]2[CH:27]=[C:28]([Cl:30])[CH:29]=[C:24]([Cl:23])[CH:25]=2)([OH:36])[C:32]([F:35])([F:34])[F:33])=[CH:12][CH:11]=1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 2305841-(4-Bromonaphthalen-1-yl)ethanoneHCID 2724682Lithium diisopropylamideHCID 27582311-(3,5-Dichlorophenyl)-2,2,2-trifluoroethan-1-one

생성물 1

HCID 866732401-(4-Bromo-1-naphthalenyl)-3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxy-1-butanone수율 40%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
3회

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온도
-78 °C

실험 절차

Lithium diisopropylamide (Aldrich Chemical Company, 2M in tetrahydrofuran/ethylbenzene, 4 mL, 7.94 mmol) was added to tetrahydrofuran (4 mL) at −78° C. A solution of 1-(4-bromo-1-naphthalenyl)ethanone (1.8 g, 7.22 mmol) in tetrahydrofuran (4 mL) was added dropwise to the mixture. When the addition was complete the mixture was stirred for 30 min at −78° C. Then a solution of 1-(3,5-dichlorophenyl)-2,2,2-trifluoroethanone (1.75 g, 7.20 mmol) in tetrahydrofuran (4 mL) was added dropwise to the mixture at such a rate that the temperature of the reaction mixture did not exceed −55° C. The mixture was allowed to warm to ambient temperature over 120 min. The mixture was then poured into 1N hydrochloric acid (100 mL) and extracted with ethyl acetate (2×100 mL). The combined extracts were dried and evaporated. Chromatography on silica gel (eluted with 1:9 ethyl acetate/hexanes) and crystallization from hexanes gave the title product as a white solid (1.1 g, 40% yield) melting at 74.5-75° C. (after recrystallization from hexanes).

후처리

  1. additionWhen the addition
  2. customdid not exceed −55° C
  3. temperatureto warm to ambient temperature over 120 min
  4. extractionextracted with ethyl acetate (2×100 mL)
  5. customThe combined extracts were dried
  6. customevaporated
  7. customChromatography on silica gel (eluted with 1:9 ethyl acetate/hexanes) and crystallization from hexanes

출처 및 근거

ORD 기록
ord-6c5b52712fda4f8aaccb0e300c5ba0d8
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08513431B2

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