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Trifluoroacetic acid → 5-Methyl-6-(piperazin-1-yl)nicotinonitrile

HRID 2411235
ノート
印刷プレビュー

反応式

HRID 2411235 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:19]([CH3:20])=[CH:18][C:17]([C:21]#[N:22])=[CH:16][N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:20][C:19]1[C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[N:15][CH:16]=[C:17]([CH:18]=1)[C:21]#[N:22]
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 6422Trifluoroacetic acidHCID 66838837Tert-butyl 4-(5-cyano-3-methylpyridin-2-yl)piperazine-1-carboxylate

生成物 1

HCID 673812745-Methyl-6-(piperazin-1-yl)nicotinonitrile収率 65.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-(5-Cyano-3-methylpyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (2.45 g) described in Preparation Example 102 was dissolved in dichloromethane (15 mL), trifluoroacetic acid (5 mL) was added, and the mixture was stirred at room temperature for 6 hr. The solvent was evaporated from the reaction mixture, aqueous potassium carbonate solution was added, and the mixture was extracted with chloroform. The solvent was evaporated from the organic layer, the obtained residue was purified by NH-coated silica gel silica gel column chromatography (hexane:ethyl acetate) to give the title compound (1.07 g).

後処理

  1. customThe solvent was evaporated from the reaction mixture, aqueous potassium carbonate solution
  2. additionwas added
  3. extractionthe mixture was extracted with chloroform
  4. customThe solvent was evaporated from the organic layer
  5. customthe obtained residue was purified by NH-coated silica gel silica gel column chromatography (hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-298508514bce4dc5a76a5cde757382a4
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08816079B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート