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Dimethylformamide → Methyl 4-bromo-3-fluorobenzeneacetate

HRID 1050136
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HRID 1050136 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][C:3]=1[F:12].O=S(Cl)Cl.[CH3:17]N(C=O)C>CO>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH3:17])=[O:10])=[CH:4][C:3]=1[F:12]
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참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 534348702-(4-Bromo-3-fluorophenyl)acetic acid

생성물 1

HCID 71265948Methyl 4-bromo-3-fluorobenzeneacetate수율 801.5%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
80 °C

실험 절차

To a mixture of 2-(4-bromo-3-fluorophenyl)acetic acid (5 g, 21.46 mmol) in MeOH (50 mL) was added SOCl2 (1.879 mL, 25.7 mmol) and DMF (0.166 mL, 2.146 mmol). Then the mixture was stirred at 80° C. for 16 h. The mixture was concentrated and extracted with EA (100 mL×2) and washed with NaHCO3 (100 mL) to give the organic layer. The combined organic extract was washed with brine, dried over Na2SO4, filtered, and concentrated to yield a brown oil of methyl 2-(4-bromo-3-fluorophenyl)acetate (5 g, 17.20 mmol, 80% yield): 1H NMR (400 MHz, MeOH-d4) δ 7.53 (t, J=7.6 Hz, 1H), 7.15 (dd, J=1.6, 9.6 Hz, 1H), 7.04-6.99 (m, 1H), 3.67 (s, 3H), 3.65 (s, 2H); ES-LCMS m/z 249.0 (M+H+2).

후처리

  1. concentrationThe mixture was concentrated
  2. extractionextracted with EA (100 mL×2)
  3. washwashed with NaHCO3 (100 mL)
  4. customto give the organic layer
  5. extractionThe combined organic extract
  6. washwas washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e890bcbf76284227bf16cd26aedd0f4d
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382238B2

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