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

HRID 551062

반응식

HRID 551062 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.[N+:10]([O-])([OH:12])=[O:11]>OS(O)(=O)=O>[Cl:1][C:2]1[C:7]([N+:10]([O-:12])=[O:11])=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1

참가 물질

4

반응물 2

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

생성물 1

HCID 2827402,6-Dichloro-3-nitropyridin-4-amine

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of 2,6-dichloro-4-aminopyridine (5.0 g, 30.6 mmol) in conc. H2SO4 (25 mL) at 0° C. in an ice-acetone bath was added 90% HNO3 (10 mL) dropwise. The reaction mixture was warmed to ambient temperature and stirred for 1 h then poured onto ice (100 g). The solid precipitate was isolated by filtration, washed with cold H2O and dried under high vacuum. The resulting solid was dissolved in conc. H2SO4 (50 mL) and heated at 100° C. for 20 min. The reaction mixture was poured onto ice (150 g) and neutralized with conc. NH4OH while maintaining the temperature below 20° C. The precipitate was isolated by filtration, washed with cold H2O, and dried to yield the title compound. MS: m/z=209 (M+1).

후처리

  1. additionthen poured onto ice (100 g)
  2. customThe solid precipitate was isolated by filtration
  3. washwashed with cold H2O
  4. customdried under high vacuum
  5. dissolutionThe resulting solid was dissolved in conc. H2SO4 (50 mL)
  6. temperatureheated at 100° C. for 20 min
  7. additionThe reaction mixture was poured onto ice (150 g)
  8. temperaturewhile maintaining the temperature below 20° C
  9. customThe precipitate was isolated by filtration
  10. washwashed with cold H2O
  11. customdried

출처 및 근거

ORD 기록
ord-bf9b0cf786734cbfa26037a8716fadfd
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947677B2

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