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Thionyl Chloride → 7-Fluorobenzofuran

HRID 1025489
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HRID 1025489 반응식
[F:1][C:2]1[C:10]2[O:9][CH2:8][CH:7](O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.O=S(Cl)Cl>N1C=CC=CC=1.C(Cl)Cl>[F:1][C:2]1[C:10]2[O:9][CH:8]=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 24386Thionyl ChlorideHCID 657217987-Fluoro-2,3-dihydrobenzofuran-3-ol

생성물 1

HCID 151587267-Fluorobenzofuran수율 235.1%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a solution of 7-fluoro-2,3-dihydrobenzofuran-3-ol (4.6 g, 29 8 mmol) in pyridine (93 mL) at 0° C. was added SOCl2 (21.7 mL, 298 mmol) dropwise. Upon completion of addition, the mixture was stirred at 0° C. for 1.5 h. At the conclusion of this period, the reaction mixture was carefully quenched with aqueous NaHCO3 (saturated, 100 mL) to reach a pH=9. Once at the prescribed pH, the reaction mixture was extracted with CH2Cl2 (4×15 mL). The combined organic layers were washed with aqueous NaHCO3 (5%, 40 mL), water (40 mL), and then concentrated to yield the crude product. The crude product was dissolved in CH2Cl2 (50 mL), washed with aqueous HCl (1 N, 5×10 mL), and then water (40 mL). The organic layer was separated, dried (MgSO4), filtered, and concentrated to afford Compound 1C as a brown oil (2.56 g). 1H NMR (500 MHz, CDCl3) δ ppm 7.67 (d, J=2.2 Hz, 1 H), 7.33-7.40 (m, 1 H), 7.17 (td, J=8.0, 4.4 Hz, 1 H), 7.04 (dd, J=10.7, 8.0 Hz, 1 H), 6.79-6.85 (m, 1 H).

후처리

  1. additionUpon completion of addition
  2. customAt the conclusion of this period, the reaction mixture was carefully quenched with aqueous NaHCO3 (saturated, 100 mL)
  3. extractionOnce at the prescribed pH, the reaction mixture was extracted with CH2Cl2 (4×15 mL)
  4. washThe combined organic layers were washed with aqueous NaHCO3 (5%, 40 mL), water (40 mL)
  5. concentrationconcentrated
  6. customto yield the crude product
  7. washwashed with aqueous HCl (1 N, 5×10 mL)
  8. customThe organic layer was separated
  9. dry with materialdried (MgSO4)
  10. filtrationfiltered
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-31dd6d92038d443d9bf2aac8df840143
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729084B2

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