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2-Amino-4-bromopyridine → HCID 58574614, 화합물

HRID 1619393
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HRID 1619393 반응식
[CH3:1][C:2]1([CH3:13])[CH2:7][CH2:6][CH:5]([C:8]([O:10]C)=O)[C:4](=O)[CH2:3]1.[Br:14][C:15]1[CH:20]=[CH:19][N:18]=[C:17]([NH2:21])[CH:16]=1>ClCCCl>[Br:14][C:15]1[CH:20]=[CH:19][N:18]2[C:17](=[N:21][C:4]3[CH2:3][C:2]([CH3:1])([CH3:13])[CH2:7][CH2:6][C:5]=3[C:8]2=[O:10])[CH:16]=1
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참가 물질

4

반응물 2

HCID 6932822-Amino-4-bromopyridineHCID 5314361Methyl 4,4-dimethyl-2-oxocyclohexane-1-carboxylate

생성물 1

HCID 58574614HCID 58574614, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A solution of methyl 4,4-dimethyl-2-oxocyclohexanecarboxylate (0.5 g, 2.7 mmol, 1 eq), 4-bromopyridin-2-amine (0.51 g, 2.97 mmol, 1.1 eq) and PPA in 1,2-dichloroethane was stirred at 80° C. for 4 hours. After it was cooled to rt, the reaction mixture was quenched with saturated Na2CO3 and extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine and dried over anhydrous sodium sulfate. After filtration and concentration, the residue was purified by silica gel chromatography to give the desired product.

후처리

  1. customthe reaction mixture was quenched with saturated Na2CO3
  2. extractionextracted with ethyl acetate (3×50 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationAfter filtration and concentration
  6. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-fa471324beb44130a7ba48fa5acba095
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772301B2

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