Acetic Anhydride → 4-(2,5-Dioxo-2,5-dihydro-1H-pyrrol-1-yl)phenyl acetate

HRID 257546

반응식

HRID 257546 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:15])/[CH:10]=[CH:11]\[C:12](O)=[O:13])=[CH:4][CH:3]=1.[C:16]([O-])(=[O:18])[CH3:17].[Na+].C(OC(=O)C)(=O)C>O>[C:16]([O:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:9](=[O:15])[CH:10]=[CH:11][C:12]2=[O:13])=[CH:4][CH:3]=1)(=[O:18])[CH3:17]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 1550903(Z)-4-((4-Hydroxyphenyl)amino)-4-oxobut-2-enoic acid

생성물 1

HCID 2276844-(2,5-Dioxo-2,5-dihydro-1H-pyrrol-1-yl)phenyl acetate수율 53%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a three-neck 1 liter reaction vessel equipped with a condenser, a teflon stirring rod and a thermometer, 97 g (0.49 moles) of N-(4-hydroxyphenyl)maleamic acid, 27.7 g (0.38 moles) of sodium acetate and 400 g of acetic anhydride are added and then heated by using silicone oil. When the reaction solution reaches 70° C. for 2 hours with stirring, the solution is poured into a large amount of distilled water and a great amount of precipitates are formed. The precipitate is taken by filtration and washed several times with distilled water to remove acetic acid, followed by recrystallization from ethanol to give the titled compound. Yield 53%. B.P. 155°-158° C.

후처리

  1. customTo a three-neck 1 liter reaction vessel
  2. customequipped with a condenser
  3. temperatureheated
  4. customa great amount of precipitates
  5. customare formed
  6. filtrationThe precipitate is taken by filtration
  7. washwashed several times with distilled water
  8. customto remove acetic acid
  9. customfollowed by recrystallization from ethanol

출처 및 근거

ORD 기록
ord-996413313eac4b079d48530336575859
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262500

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