Nitric Acid → 2,5-Dichloro-4-nitro-1-oxo-1lambda~5~-pyridine

HRID 895572ノート

反応式

HRID 895572 の反応式
OS(O)(=O)=O.O=S(=O)=O.[N+:10]([O-:13])(O)=[O:11].[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][N+:16]=1[O-:22]>OS(O)(=O)=O>[Cl:14][C:15]1[CH:20]=[C:19]([N+:10]([O-:13])=[O:11])[C:18]([Cl:21])=[CH:17][N+:16]=1[O-:22]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 24681Fuming sulfuric acidHCID 113326572,5-Dichloro-pyridine 1-oxide

生成物 1

HCID 222840452,5-Dichloro-4-nitro-1-oxo-1lambda~5~-pyridine

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

At 0° C., 30% oleum (13 mL) is added slowly to fuming HNO3 (22 mL) and the resulting mixture is added slowly to the solution of 2,5-dichloro-pyridine 1-oxide (5.2 g, 31 mmol) in concentrated H2SO4. After addition, the reaction mixture is warmed to room temperature over 1 hr. then heated to 80° C. for 2 hr. After cooling to room temperature, the mixture is poured into ice (120 g) and precipitate is formed gradually. The solid is collected by filtration and washed with water. The product is obtained as yellow solid. 1H NMR (CDC3) δ 8.46 (s, 1H), 8.25 (s, 1H).

後処理

  1. additionAfter addition
  2. temperaturethen heated to 80° C. for 2 hr
  3. temperatureAfter cooling to room temperature
  4. customprecipitate is formed gradually
  5. filtrationThe solid is collected by filtration
  6. washwashed with water
  7. customThe product is obtained as yellow solid

出典と根拠

ORDレコード
ord-6dc3d4b992e34ef9a58ce301e53e0713
出典データセット
uspto-grants-2005_07
特許番号
US06916819B2

反応ノート

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