Pyridine → HCID 23373914、化合物

HRID 375695

反応式

HRID 375695 の反応式
[CH:1]1[CH:6]=[C:5]2[C:7](S(O)(=O)=O)=[CH:8][C:9]([OH:12])=[C:10]([NH2:11])[C:4]2=[CH:3][CH:2]=1.N1[CH:22]=[CH:21]C=CC=1.C(OC(=O)C)(=O)C.[S:30](=O)(=[O:33])([OH:32])[OH:31]>O>[CH3:21][C:22]1[O:12][C:9]2[CH:8]=[CH:7][C:5]3[C:4](=[CH:3][C:2]([S:30]([OH:33])(=[O:32])=[O:31])=[CH:1][CH:6]=3)[C:10]=2[N:11]=1

参加物

6

反応物 4

HCID 1049PyridineHCID 1118Sulfuric AcidHCID 7918Acetic Anhydride2 回HCID 83161-Amino-2-naphthol-4-sulfonic acid

生成物 1

HCID 23373914HCID 23373914、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

(1 mole) of 1-amino-2-naphthol-4-sulfonic acid and 80 ml of pyridine are mixed and this mixture is then dissolved by adding 30 ml water. The amber colored solution is then heated gently in a heating jacket and 360 ml of acetic anhydride are added in small fractions. During this addition, a large amount of heat is evolved, causing the mixture to reflux vigorously. After the addition of the acetic anhydride is complete, the mixture is heated under reflux for 2 hours. By removing the solvents under reduced pressure, a thick syrup is obtained which is dissolved in 500 ml water. The aqueous solution is then rendered strongly acid to universal indicator paper by adding concentrated sulfuric acid, with stirring. The product thereupon precipitated from the solution in the form of a white solid. The solid is collected by filtration, washed with water and dried. After two recrystallizations from ethyl alcohol, 35 g (67%) of a white solid, melting above 320° C. are obtained.

後処理

  1. dissolutionthis mixture is then dissolved
  2. additionare added in small fractions
  3. additionDuring this addition
  4. temperaturea large amount of heat
  5. temperatureto reflux vigorously
  6. temperaturethe mixture is heated
  7. temperatureunder reflux for 2 hours
  8. customBy removing the solvents under reduced pressure
  9. customa thick syrup is obtained which
  10. customThe product thereupon precipitated from the solution in the form of a white solid
  11. filtrationThe solid is collected by filtration
  12. washwashed with water
  13. customdried
  14. customAfter two recrystallizations from ethyl alcohol, 35 g (67%) of a white solid
  15. custommelting above 320° C.
  16. customare obtained

出典と根拠

ORDレコード
ord-8802befc33604483b716124f29246cbe
出典データセット
uspto-grants-1996_01
特許番号
US05486616

関連ノート

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