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3-Bromo-5-fluorobenzotrifluoride → benzyl {(2S)-1-[3-fluoro-5-(trifluoromethyl)phenyl]-1-oxopropan-2-yl}carbamate

HRID 1508589
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HRID 1508589 반응식
CON(C)[C:4](=[O:18])[C@@H:5]([NH:7][C:8](=[O:17])[O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH3:6].Br[C:21]1[CH:22]=[C:23]([C:28]([F:31])([F:30])[F:29])[CH:24]=[C:25]([F:27])[CH:26]=1.C([Mg]Cl)(C)C>C1COCC1.[Cl-].[Na+].O>[F:27][C:25]1[CH:26]=[C:21]([C:4](=[O:18])[C@@H:5]([NH:7][C:8](=[O:17])[O:9][CH2:10][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH3:6])[CH:22]=[C:23]([C:28]([F:29])([F:30])[F:31])[CH:24]=1
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참가 물질

6

반응물 3

HCID 27363233-Bromo-5-fluorobenzotrifluorideHCID 10515879(S)-Benzyl 1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamateHCID 178418918HCID 178418918, 화합물

생성물 1

HCID 86704637benzyl {(2S)-1-[3-fluoro-5-(trifluoromethyl)phenyl]-1-oxopropan-2-yl}carbamate

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 57417360
Sodium chloride; water
용매

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온도
-20 °C

실험 절차

To a solution of the commercially available benzyl {(2S)-1-[methoxy(methyl)amino]-1-oxopropan-2-yl}carbamate (5.48 g, 20.58 mmol) and 3-bromo-5-fluorobenzotrifluoride (5 g, 20.58 mmol) in THF (52 ml) at −30° C. was added isopropylmagnesium chloride (20.58 ml, 41.2 mmol) dropwise under nitrogen. Removed the cold bath and allowed the reaction to age overnight to ambient temperature. The crude was cooled to −20° C. followed by addition of HC (1N, ice bath cold). The resulting mixture was worked up with brine, extracted with ethyl acetate, dried over Na2SO4, filtered and evaporated. The pot residue was purified by flash chromatography (SiO2, Biotage 65i cartridge). The column was eluted by an ethyl acetate/hexanes mixture (0% to 40% ethyl acetate). Related fractions were pooled and evaporated under reduced pressure to afford a yellow oil of 5.4655 g as the titled compound. 1H-NMR (CDCl3, 500 MHz) δ 8.03 (s, 1H), 7.86 (d, J=8.5 Hz, 1H), 7.57 (d, J=8 Hz, 1H), 7.38-7.30 (m, 5H), 5.7 (d, J=7.5 Hz, 1H), 5.3 (ps quintet, J=7.5 Hz, 1H), 1.45 (d, J=7 Hz, 3H).

후처리

  1. customRemoved the cold bath
  2. customthe reaction to age overnight to ambient temperature
  3. additionfollowed by addition of HC (1N, ice bath cold)
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe pot residue was purified by flash chromatography (SiO2, Biotage 65i cartridge)
  9. washThe column was eluted by an ethyl acetate/hexanes mixture (0% to 40% ethyl acetate)
  10. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-1492c68e01c24dbeaf291884ebd83c24
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221834B2

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