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

HRID 510024ノート

反応式

HRID 510024 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 27740222,6-Dichloro-5-fluoronicotinamide

反応条件

温度
62.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4c552e517d324b67a49cc6f9842de255
出典データセット
uspto-grants-2015_08
特許番号
US09096592B2

反応ノート

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