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2-Bromopyridine → N-(2-(4-fluorophenyl)-2-methylpropyl)-6-(pyridin-2-yl)pyridazin-3-amine

HRID 869150
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HRID 869150 반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.C(OB(OC(C)C)OC(C)C)(C)C.[Li]CCCC.Cl[C:27]1[N:32]=[N:31][C:30]([NH:33][CH2:34][C:35]([C:38]2[CH:43]=[CH:42][C:41]([F:44])=[CH:40][CH:39]=2)([CH3:37])[CH3:36])=[CH:29][CH:28]=1.P(C(C)(C)C)(C(C)(C)C)(C(C)(C)C)=O.[F-].[K+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].O1CCOCC1.C1(C)C=CC=CC=1.C1COCC1>[F:44][C:41]1[CH:40]=[CH:39][C:38]([C:35]([CH3:37])([CH3:36])[CH2:34][NH:33][C:30]2[N:31]=[N:32][C:27]([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=3)=[CH:28][CH:29]=2)=[CH:43][CH:42]=1
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참가 물질

10

반응물 6

HCID 79732-BromopyridineHCID 21531Triisopropyl borateHCID 522689Potassium FluorideHCID 10927323Tri-tert-butylphosphine oxideHCID 866861256-Chloro-N-(2-(4-fluorophenyl)-2-methylpropyl)pyridazin-3-amineHCID 178418339Butyllithium

생성물 1

HCID 67452706
N-(2-(4-fluorophenyl)-2-methylpropyl)-6-(pyridin-2-yl)pyridazin-3-amine
수율 6.2%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 312751,4-Dioxane용매HCID 22635083Tetrahydrofuran toluene용매

반응 조건

온도
-78 °C

실험 절차

To a 25 mL round bottom flask was added 2-bromopyridine (500 mg, 3.2 mmol, 1.0 equiv), triisopropylborate (654 mg, 3.5 mmol, 1.1 equiv), and an 80% toluene/THF mixture (16 mL). The mixture was cooled to −78° C. After stirring for 10 min, n-BuLi (1.7 mL, 3.48 mmol, 1.1 equiv of a 2.0 M/hexanes solution) was slowly added over an hour. After the addition was complete, the reaction mixture was stirred for 30 min and allowed to warm to rt and stirred overnight. The reaction was then concentrated at 100° C. and dried in vacuo for 2 h. To 100 mg of this crude solid in a microwave vial was added 6-chloro-N-(2-(4-fluorophenyl)-2-methylpropyl)pyridazin-3-amine (70 mg, 0.25 mmol), Pd2 dba3 (10 mg, 0.011 mmol), PO(tBu)3 (5 mg, 0.030 mmol), potassium fluoride (43 mg, 0.75 mmol), and dioxane (0.75 mL). The reaction was degassed with nitrogen for 5 minutes and then heated in a microwave reactor at 160° C. for 15 min. The reaction was then concentrated, dissolved in EtOAc (25 mL), washed with water, dried over Na2SO4, filtered, concentrated, and purified by reverse phase column chromatography to give 5 mg of N-(2-(4-fluorophenyl)-2-methylpropyl)-6-(pyridin-2-yl)pyridazin-3-amine as a white solid. m/z=323.1 [M+H]+.

후처리

  1. additionAfter the addition
  2. stirringthe reaction mixture was stirred for 30 min
  3. temperatureto warm to rt
  4. stirringstirred overnight
  5. concentrationThe reaction was then concentrated at 100° C.
  6. customdried in vacuo for 2 h
  7. customThe reaction was degassed with nitrogen for 5 minutes
  8. temperatureheated in a microwave reactor at 160° C. for 15 min
  9. concentrationThe reaction was then concentrated
  10. dissolutiondissolved in EtOAc (25 mL)
  11. washwashed with water
  12. dry with materialdried over Na2SO4
  13. filtrationfiltered
  14. concentrationconcentrated
  15. custompurified by reverse phase column chromatography

출처 및 근거

ORD 기록
ord-5c629727c3974d0fa6dfc41b950ce42a
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969346B2

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