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Sodium Bicarbonate → 6-(Oxan-4-yl)pyridin-3-amine

HRID 1748499
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HRID 1748499 반응식
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].F[B-](F)(F)F.C(P(C(C)(C)C)C(C)(C)C)(C)(C)C.Br[C:30]1[CH:31]=[CH:32][C:33]([CH:36]2[CH2:41][CH2:40][O:39][CH2:38][CH2:37]2)=[N:34][CH:35]=1.[F-].C([N+:47](CCCC)(CCCC)CCCC)CCC.C(=O)(O)[O-].[Na+]>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].O1CCCC1.C1(C)C=CC=CC=1>[O:39]1[CH2:40][CH2:41][CH:36]([C:33]2[N:34]=[CH:35][C:30]([NH2:47])=[CH:31][CH:32]=2)[CH2:37][CH2:38]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 516892Sodium BicarbonateHCID 2724141Tetrabutylammonium FluorideHCID 2733832Lithium hexamethyldisilazaneHCID 225027355-bromo-2-(tetrahydro-2H-pyran-4-yl)pyridineHCID 44558591Tri-t-butylphosphine fluoroborate

생성물 1

HCID 866924516-(Oxan-4-yl)pyridin-3-amine

시약·촉매·용매

3
HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 1140Toluene용매2회HCID 8028Tetrahydrofuran용매

실험 절차

After 1.0M toluene-solution (9.8 ml) of lithium bis(trimethylsilyl)amide was added to bis(dibenzylideneacetone)palladium (0) (67 mg) and tri-tert-butylphosphine tetrafluoroborate (118 mg) at 70° C. under an atmosphere of nitrogen, a toluene solution (8.2 ml) of 5-bromo-2-(tetrahydro-2H-pyran-4-yl)pyridine (1.97 g) was added dropwise and stirred at the same temperature for 0.5 hour. Next, the reaction solution was cooled to room temperature, 1.0M tetrahydrofuran-solution (7.0 ml) of tetrabutylammonium fluoride was added and stirred at the same temperature for 1.5 hours. After completion of the reaction, a saturated aqueous solution of sodium bicarbonate was added and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated. The resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate) to give the titled compound (1.1 g) as a white solid.

후처리

  1. stirringstirred at the same temperature for 1.5 hours
  2. customAfter completion of the reaction
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-9f7957d5786a4d1384289942c085bd20
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150555B2

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