Hydrochloric Acid → HCID 178526838, 화합물

HRID 601481

반응식

HRID 601481 반응식
Cl.[OH:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][N:4]=1.[Cl:12]([O-])(=O)=O.[K+]>O>[Cl:12][C:8]1[C:3]([OH:2])=[N:4][CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[CH:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6426889Potassium ChlorateHCID 178526703HCID 178526703, 화합물

생성물 1

HCID 178526838HCID 178526838, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
53 °C

실험 절차

Concentrated hydrochloric acid (239 g) was added to 2-hydroxy-5-nitropyridine (40.0 g). The resulting slurry was heated to 53° C., and stirred until all the solids dissolved. To this was slowly added a solution of potassium chlorate (14.0 g) in water (250 g), while maintaining the temperature between 55° C. and 59° C. The resulting mixture was stirred at 58-62° C. for about 1 hour. The reaction was then cooled to room temperature, stirred for 12 hours and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/DMSO-d6) δ 8.64 (d, J=2.9 Hz, 1H), 8.35 (d, J=2.9 Hz, 1H)

후처리

  1. dissolutiondissolved
  2. temperaturewhile maintaining the temperature between 55° C. and 59° C
  3. stirringThe resulting mixture was stirred at 58-62° C. for about 1 hour
  4. temperatureThe reaction was then cooled to room temperature
  5. stirringstirred for 12 hours
  6. filtrationfiltered
  7. washAfter washing the wet cake with water
  8. customthe product was dried in a vacuum oven

출처 및 근거

ORD 기록
ord-492c546b2d804bae9106948c18fa0755
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902371B2

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