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Methyl iodide → 7-Chloro-2-methyl-furo[3,2-B]pyridine

HRID 503592
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HRID 503592 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9](I)[O:10][C:3]=12.[Li][CH2:13]CCC.CI.S([O-])([O-])(=O)=O.[Mg+2]>C1COCC1>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([CH3:13])[O:10][C:3]=12
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참가 물질

6

반응물 4

HCID 6328Methyl iodide2회HCID 24083Sulfuric acid magnesium salt (1:1)HCID 66779473HCID 66779473, 화합물HCID 178418339Butyllithium

생성물 1

HCID 108448217-Chloro-2-methyl-furo[3,2-B]pyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In an oven-dried round bottom flask, 7-chloro-2-iodofuro[3,2-b]pyridine (0.200 g, 0.72 mmol) was dissolved in 3 mL THF and cooled to −78° C. nBuLi (0.43 ml, 1.1 mmol) was slowly added and the reaction was stirred for one hour. Meanwhile, a vial was filled with MeI and warmed to RT. Magnesium sulfate was added and the mixture was stirred for 5 minutes and filtered into another vial. Immediately from this vial, MeI (0.11 ml, 1.8 mmol) was added to the reaction which was stirred at −78° C. for 3 hours. The reaction was quenched with saturated ammonium chloride solution and warmed to RT. DCM was added, the layers were separated, and the aqueous layer was extracted twice with DCM. The combined organic layers were dried with sodium sulfate, filtered, and concentrated. The material was purified via column chromatography (gradient elution 0-50% EtOAc:Hex) to afford 7-chloro-2-methylfuro[3,2-b]pyridine as a light brown oil. MS: M+H+=168.3.

후처리

  1. additionwas slowly added
  2. stirringthe mixture was stirred for 5 minutes
  3. filtrationfiltered into another vial
  4. stirringwas stirred at −78° C. for 3 hours
  5. customThe reaction was quenched with saturated ammonium chloride solution
  6. temperaturewarmed to RT
  7. additionDCM was added
  8. customthe layers were separated
  9. extractionthe aqueous layer was extracted twice with DCM
  10. dry with materialThe combined organic layers were dried with sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated
  13. customThe material was purified via column chromatography (gradient elution 0-50% EtOAc:Hex)

출처 및 근거

ORD 기록
ord-7838fc646596462c8dbd3bc10aa3d760
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776857B2

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