Nitric Acid → 2,6-Dichloro-3-nitropyridin-4-amine

HRID 343779

反応式

HRID 343779 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([Cl:9])[CH:3]=1.[N+:10]([O-])([OH:12])=[O:11].[OH-].[Na+]>OS(O)(=O)=O>[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([Cl:9])[C:3]=1[N+:10]([O-:12])=[O:11]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 14798Sodium HydroxideHCID 1376524-Amino-2,6-dichloropyridine

生成物 1

HCID 2827402,6-Dichloro-3-nitropyridin-4-amine収率 77.1%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
55 °C

実験手順

To a solution of 4-amino-2,6-dichloropyridine (1.07 g, 6.56 mmol) in conc H2SO4 (3.5 mL) was added 0.50 mL of 70% HNO3 (7.94 mmol) at room temperature. The mixture was stirred at 55° C. for 15 h, then poured into ice-H2O (70 mL). To this mixture was added 40% aq. NaOH slowly to adjust the pH to 10. The precipitate was filtered, washed with water and dried to give 1.052 g (77%) of 23 as a pale yellow powder, mp 136°-8° C. 1H NMR (CDCl3) δ 6.116 (bs, 2H), 6.750 (s, 1H). It was used for the next reaction without further purification.

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-f42a47440d0d4083baed06e27cdd7727
出典データセット
uspto-grants-1999_01
特許番号
US05863916

関連ノート

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