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Bromine → 6-Bromo-2-nitropyridin-3-amine

HRID 627308
ノート
印刷プレビュー

反応式

HRID 627308 の反応式
[N+:1]([C:4]1[C:9]([NH2:10])=[CH:8][CH:7]=[CH:6][N:5]=1)([O-:3])=[O:2].C([O-])(=O)C.[Na+].[Br:16]Br>C(O)(=O)C>[Br:16][C:6]1[N:5]=[C:4]([N+:1]([O-:3])=[O:2])[C:9]([NH2:10])=[CH:8][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24408BromineHCID 832812-Nitropyridin-3-amineHCID 517045Sodium Acetate

生成物 1

HCID 565878066-Bromo-2-nitropyridin-3-amine収率 64.3%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
0 °C

実験手順

To a stirred suspension of 2-nitro-pyridin-3-ylamine (5.06 g, 36.40 mmol) and sodium acetate (2.99 g, 36.46 mmol) in acetic acid (40 mL), a solution of bromine (2.5 mL, 48.79 mmol) in acetic acid (8 ml) was added drop-wise and the reaction mixture was stirred overnight. The acetic acid was removed under reduced pressure. The residue was cooled to 0° C., neutralized with saturated sodium bicarbonate solution to adjust the pH to ˜7, and extracted with ethyl acetate (4×50 mL). The combined organic extracts were washed with brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The residue was triturated with ethyl acetate to afford compound (5) (5.1 g) as a yellow solid.

後処理

  1. customThe acetic acid was removed under reduced pressure
  2. extractionextracted with ethyl acetate (4×50 mL)
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was triturated with ethyl acetate

出典と根拠

ORDレコード
ord-3f601925248643048203571bed82ebba
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309267B2

反応ノート

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