Nitric Acid → 2,6-Dichloro-4-nitraminopyridine

HRID 81202

반응식

HRID 81202 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.OS(O)(=O)=O.[N+:15]([O-])([OH:17])=[O:16]>>[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][N+:15]([O-:17])=[O:16])[CH:5]=[C:4]([Cl:9])[N:3]=1

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 1376524-Amino-2,6-dichloropyridine

생성물 1

HCID 4216172,6-Dichloro-4-nitraminopyridine

반응 조건

온도
0 °C

실험 절차

2,6-dichloropyridin-4-amine (100 g, 0.617 mol) was added slowly to conc. H2SO4 (415 mL) by portion while cooled with an ice bath. The mixture was cooled to 0° C., and nitric acid (250 mL) was added dropwise at 0° C. The mixture was stirred at room temperature for 2 h. TLC (petroleum ether/ethyl acetate=2:1) showed the reaction was complete. The mixture was poured into crushed ice and stirred for 30 min. The resulting precipitate was collected by filtration and washed with water to give crude N-(2,6-dichloropyridin-4-yl)nitramide as a yellow solid, which was used for the next step without further purification.

후처리

  1. temperaturewhile cooled with an ice bath
  2. additionThe mixture was poured
  3. custominto crushed ice
  4. stirringstirred for 30 min
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with water

출처 및 근거

ORD 기록
ord-05adcfb6810f41fbbbef635f537c4b81
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846657B2

연결된 노트

불러오는 중…