Sulfuric Acid → 2,6-Dichloro-5-fluoronicotinamide

HRID 510024노트

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HRID 510024 반응식
[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([F:10])=[C:4]([Cl:11])[N:3]=1.S(=O)(=O)(O)[OH:13]>>[Cl:1][C:2]1[N:3]=[C:4]([Cl:11])[C:5]([F:10])=[CH:6][C:7]=1[C:8]([NH2:9])=[O:13]

참가 물질

3

반응물 2

HCID 1118Sulfuric AcidHCID 27338492,6-Dichloro-5-fluoro-3-pyridinecarbonitrile

생성물 1

HCID 27740222,6-Dichloro-5-fluoronicotinamide

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온도
62.5 °C

실험 절차

A suspension of 25 g (130.90 mmol) of 2,6-dichloro-5-fluoro-3-cyanopyridine in conc. sulfuric acid (125 ml) was stirred at 60-65° C. for 1 h. After cooling to RT, the contents of the flask were poured onto ice-water and extracted three times with ethyl acetate (100 ml each time). The combined organic phases were washed with water (100 ml) and then with saturated aqueous sodium hydrogencarbonate solution (100 ml), dried and concentrated on a rotary evaporator. The material obtained was dried under high vacuum.

후처리

  1. temperatureAfter cooling to RT
  2. additionthe contents of the flask were poured onto ice-water
  3. extractionextracted three times with ethyl acetate (100 ml each time)
  4. washThe combined organic phases were washed with water (100 ml)
  5. dry with materialwith saturated aqueous sodium hydrogencarbonate solution (100 ml), dried
  6. concentrationconcentrated on a rotary evaporator
  7. customThe material obtained
  8. customwas dried under high vacuum

출처 및 근거

ORD 기록
ord-4c552e517d324b67a49cc6f9842de255
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096592B2

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