Acetic Acid → 4-Amino-5-bromopyridine-3-carboxylic acid

HRID 520469

反応式

HRID 520469 の反応式
[NH2:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[CH:4][CH:3]=1.C(O)(=O)C.[Br:15]Br>O>[NH2:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[CH:4][C:3]=1[Br:15]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24408BromineHCID 3199794-Aminonicotinic acid

生成物 1

HCID 215304944-Amino-5-bromopyridine-3-carboxylic acid収率 84%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
75 °C

実験手順

A sealed tube was charged with 4-aminonicotinic acid 45 (8.00 g, 57.9 mmol), acetic acid (75 mL) and water (75 mL). The reaction was heated at 75° C. and stirred vigorously until homogeneous. After cooling to 50° C., bromine (10.0 mL, 195 mmol) was added and stirring continued for 16 h. Upon cooling to 0° C., the resulting orange precipitate was collected by filtration, rinsed with H2O, and dried under vacuum to give 46 (10.5 g, 84% yield).

後処理

  1. temperatureAfter cooling to 50° C.
  2. stirringstirring
  3. temperatureUpon cooling to 0° C.
  4. filtrationthe resulting orange precipitate was collected by filtration
  5. washrinsed with H2O
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-e6fe524ad1694ba8934cf5ce81187a03
出典データセット
uspto-grants-2016_05
特許番号
US09326986B2

関連ノート

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