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2-Amino-4-bromopyridine → HCID 58574614、化合物

HRID 1619393
ノート
印刷プレビュー

反応式

HRID 1619393 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 58574614HCID 58574614、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fa471324beb44130a7ba48fa5acba095
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772301B2

反応ノート

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