Pyridine → HCID 23373914, 화합물

HRID 375695

반응식

HRID 375695 반응식
[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

참가 물질

6

반응물 4

HCID 1049PyridineHCID 1118Sulfuric AcidHCID 7918Acetic Anhydride2회HCID 83161-Amino-2-naphthol-4-sulfonic acid

생성물 1

HCID 23373914HCID 23373914, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

(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.

후처리

  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

출처 및 근거

ORD 기록
ord-8802befc33604483b716124f29246cbe
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05486616

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