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Iodine chloride → HCID 59838025, 화합물

HRID 1438133
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HRID 1438133 반응식
[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[O:12][CH3:13])(=[O:3])[CH3:2].[I:14]Cl>C(Cl)Cl>[C:1]([O:4][C:5]1[CH:10]=[C:9]([I:14])[C:8]([F:11])=[CH:7][C:6]=1[O:12][CH3:13])(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24640Iodine chlorideHCID 59838040HCID 59838040, 화합물

생성물 1

HCID 59838025HCID 59838025, 화합물수율 85.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
50 °C

실험 절차

To a solution of 64A (850 mg, 4.6 mmol) in CH2Cl2 (5.0 mL) was added ICl (1.0 M in CH2Cl2, 10.2 mL, 10.2 mmol). The mixture was stirred at 50° C. for 4 h and then at rt for 18 h. The reaction was quenched by a sat. solution of NaHCO3. After extraction with CH2Cl2, the organic layer was washed with a solution of Na2S2O3, brine and dried over Na2SO4. After evaporation of the solvent, the crude product was purified by column chromatography (EtOAc:hexanes=1:4) to give 64B (1.22 g, 80% yield) as a solid. 1H NMR (400 MHz, CDCl3) δ ppm 2.29 (s, 3H) 3.81 (s, 3H) 6.73 (d, J=9.23 Hz, 1H) 7.35 (d, J=6.59 Hz, 1H).

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후처리

  1. waitat rt for 18 h
  2. customThe reaction was quenched by a sat. solution of NaHCO3
  3. extractionAfter extraction with CH2Cl2
  4. washthe organic layer was washed with a solution of Na2S2O3, brine
  5. dry with materialdried over Na2SO4
  6. customAfter evaporation of the solvent
  7. customthe crude product was purified by column chromatography (EtOAc:hexanes=1:4)

출처 및 근거

ORD 기록
ord-5c92930ee2fd47b69a2e12ba6195a789
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622585B2

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