N-(4-Nitrophenyl)pyridin-2-amine → N-pyridin-2-yl-benzene-1,4-diamine

HRID 450065ノート

反応式

HRID 450065 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[CH:6][CH:5]=1)([O-])=O>C(OCC)(=O)C>[N:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[NH:10][C:7]1[CH:8]=[CH:9][C:4]([NH2:1])=[CH:5][CH:6]=1

参加物

3

反応物 1

HCID 12695755N-(4-Nitrophenyl)pyridin-2-amine

生成物 1

HCID 10375156N-pyridin-2-yl-benzene-1,4-diamine収率 33.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of (4-nitro-phenyl)-pyridin-2-yl-amine (280 mg, 1.3 mmol) in ethyl acetate (10 ml) was added stannous chloride dihydrate (1.17 g, 5.2 mmol) and stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate and washed with 10% sodium hydroxide solution. The organic layer was separated, washed with brine, dried and evaporated to dryness. Purification by column chromatography using ethyl acetate/hexane (2:3) yielded N-pyridin-2-yl-benzene-1,4-diamine (80 mg, 33%).

後処理

  1. washwashed with 10% sodium hydroxide solution
  2. customThe organic layer was separated
  3. washwashed with brine
  4. customdried
  5. customevaporated to dryness
  6. customPurification by column chromatography

出典と根拠

ORDレコード
ord-20b74450bf6e4cebb4f88ac854b99de8
出典データセット
uspto-grants-2013_07
特許番号
US08486962B2

反応ノート

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