Potassium Nitrate → 4-Chloro-3-iodo-5-nitropyridin-2-amine

HRID 1969795ノート

反応式

HRID 1969795 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:9].[N+:10]([O-])([O-:12])=[O:11].[K+]>OS(O)(=O)=O>[Cl:1][C:2]1[C:7]([N+:10]([O-:12])=[O:11])=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:9]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 229365964-Chloro-3-iodopyridin-2-amine

生成物 1

HCID 585571744-Chloro-3-iodo-5-nitropyridin-2-amine収率 47%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
0 °C

実験手順

A solution of 4-chloro-3-iodopyridin-2-amine (4.00 g, 15.7 mmol, Adesis) in concd H2SO4 (45 mL) was cooled to about 0° C. in an ice bath. Potassium nitrate (3.50 g, 34.6 mmol) was added in four portions over about 10 min. The resulting solution was stirred at about 0° C. for about 1 h, then at ambient temperature for about 4 h. The reaction mixture was slowly poured over crushed ice (total volume 1 L) resulting in formation of a solid that was collected by vacuum filtration and dried under vacuum to give 4-chloro-3-iodo-5-nitropyridin-2-amine (2.2 g, 47%) as a yellow solid: LC/MS (Table 1, Method c) Rt=1.48 min; MS m/z 298 (M−H)−.

後処理

  1. waitat ambient temperature for about 4 h
  2. additionThe reaction mixture was slowly poured
  3. customover crushed ice (total volume 1 L)
  4. customresulting in formation of a solid
  5. filtrationthat was collected by vacuum filtration
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-34211e888e8c4ac6bd8353791b8f8d4c
出典データセット
uspto-grants-2013_04
特許番号
US08426411B2

反応ノート

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