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Nitric Acid → 4-nitro-3-cyanopyridine N-oxide

HRID 1734217
ノート
印刷プレビュー

反応式

HRID 1734217 の反応式
[N+:1]([O-:4])(O)=[O:2].[C:5]([C:7]1[CH:8]=[N+:9]([O-:13])[CH:10]=[CH:11][CH:12]=1)#[N:6].[N+]([O-])([O-])=O.[K+]>>[N+:1]([C:12]1[CH:11]=[CH:10][N+:9]([O-:13])=[CH:8][C:7]=1[C:5]#[N:6])([O-:4])=[O:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 944Nitric AcidHCID 24434Potassium NitrateHCID 84686Nicotinonitrile 1-oxide

生成物 1

HCID 537498984-nitro-3-cyanopyridine N-oxide

反応条件

温度
100 °C

実験手順

One hundred fifty mL of stirred 15% fuming nitric acid is cooled to 5°-10° C., and 20.4 grams (0.17 mole) of 3-cyanopyridine N-oxide is added portionwise. Upon completion of addition, the reaction mixture is stirred for about 15 minutes, and then 34.4 grams (0.340 mole) of potassium nitrate is added portionwise. Upon completion of addition, the reaction mixture is warmed to about 100° C. where it is stirred for six hours. The reaction mixture is then poured into about 1000 mL of ice-water. The mixture is stirred until the ice melts, and then the resultant solid is collected by filtration. The solid is dried under reduced pressure at about 100° C., yielding 4-nitro-3-cyanopyridine N-oxide.

後処理

  1. temperatureis cooled to 5°-10° C.
  2. additionUpon completion of addition
  3. additionUpon completion of addition
  4. stirringis stirred for six hours
  5. filtrationthe resultant solid is collected by filtration
  6. customThe solid is dried under reduced pressure at about 100° C.

出典と根拠

ORDレコード
ord-5546ce4f90604ffe805f3e73f28ec3e6
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05532370

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート