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

HRID 1594102노트

반응식

HRID 1594102 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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 (CDCl3) δ 8.46 (s, 1H), 8.25 (s, 1H).

후처리

  1. additionAfter addition
  2. temperatureheated 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

출처 및 근거

ORD 기록
ord-b9cc95033a43462797c113ebec93a7ce
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07300945B2

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