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Hydrochloric Acid → 3-(2,4-Difluorophenyl)sulfanylpropan-1-ol

HRID 600547
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HRID 600547 반응식
Cl.[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[S:10][CH2:11][CH2:12][CH2:13][O:14]C1CCCCO1>CO>[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[S:10][CH2:11][CH2:12][CH2:13][OH:14]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 576632252-[3-(2,4-Difluorophenyl)sulfanylpropoxy]oxane2회

생성물 1

HCID 433923683-(2,4-Difluorophenyl)sulfanylpropan-1-ol수율 99.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1M Hydrochloric acid (170 mL) was added to a solution of 2-[3-(2,4-difluorophenyl)sulfanylpropoxy]oxane (Intermediate 26) (10.8 g, 37 mmol) in methanol (170 mL) and stirred at ambient temperature for 40 minutes. The methanol was removed under reduced pressure and the remaining aqueous phase taken to pH 6. The solution was extracted with ethyl acetate (3×50 mL) and the combined organics washed with brine (50 mL), dried (MgSO4) and the solvent removed under reduced pressure to afford the product (7.5 g, 99%). 1H NMR δ (400 MHz, CDCl3): 1.38 (t, 1H), 1.83 (quintet, 2H), 2.97 (t, 2H), 3.77 (q, 2H), 6.81-6.87 (m, 2H), 7.38-7.45 (m, 1H).

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후처리

  1. customThe methanol was removed under reduced pressure
  2. extractionThe solution was extracted with ethyl acetate (3×50 mL)
  3. washthe combined organics washed with brine (50 mL)
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-7838517c257f43efac0eda19954ef813
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902200B2

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