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Propargyl bromide → 6-Cyclopropyl-4-methoxy-3-(2-methylphenoxy)pyridazine

HRID 1821682
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HRID 1821682 반응식
[CH:1]12BC(C[CH2:7][CH2:8]1)CCC2.C(Br)C#C.[OH-].[Na+].Cl[C:17]1[N:22]=[N:21][C:20]([O:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[CH3:30])=[C:19]([O:31][CH3:32])[CH:18]=1>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O.O1CCCC1>[CH:7]1([C:17]2[N:22]=[N:21][C:20]([O:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[CH3:30])=[C:19]([O:31][CH3:32])[CH:18]=2)[CH2:8][CH2:1]1
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참가 물질

8

반응물 4

HCID 7842Propargyl bromideHCID 14798Sodium HydroxideHCID 789669-Borabicyclo(3.3.1)nonaneHCID 229401366-Chloro-4-methoxy-3-(2-methylphenoxy)pyridazine

생성물 1

HCID 229400116-Cyclopropyl-4-methoxy-3-(2-methylphenoxy)pyridazine수율 70.7%

시약·촉매·용매 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
촉매
HCID 962Water용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a tetrahydrofuran solution (2.94 mL) containing of 9-borabicyclo[3.3.1]nonane (0.5 mol/l, 1.47 mmol) was added 87.5 mg (0.735 mmol) of propargyl bromide, and the resulting mixture was refluxed for 2 hours. The reaction mixture was cooled to room temperature, 0.74 mL (2.2 mmol) of 3 mol/L aqueous sodium hydroxide solution was added to the mixture, and the resulting mixture was stirred at room temperature for 70 minutes. To the mixture were successively added 168 mg (0.669 mmol) of 6-chloro-4-methoxy-3-(2-methylphenoxy)pyridazine obtained in Example 2 (1) and 38.7 mg (0.00334 mmol) of tetrakis(triphenylphosphine)-palladium, and the resulting mixture was refluxed overnight. The reaction mixture was allowed to stand for cooling, water was added to the mixture, and the resulting mixture was extracted with ethyl acetate. The organic layers were combined, and washed successively with water and brine. After drying over anhydrous sodium sulfate, the solvent was removed. The obtained residue was purified by silica gel column chromatography to obtain 121 mg (0.473 mmol, Yield: 70.1%) of 6-cyclopropyl-4-methoxy-3-(2-methylphenoxy)pyridazine.

후처리

  1. temperaturethe resulting mixture was refluxed for 2 hours
  2. temperaturethe resulting mixture was refluxed overnight
  3. temperaturefor cooling
  4. extractionthe resulting mixture was extracted with ethyl acetate
  5. washwashed successively with water and brine
  6. dry with materialAfter drying over anhydrous sodium sulfate
  7. customthe solvent was removed
  8. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-51ed4ad8abbb44028d3d22303f3ac1df
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07608563B2

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