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Acetic Acid → HCID 12274185, 화합물

HRID 1579442
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HRID 1579442 반응식
C(C[C:4]1[CH:5]=[CH:6][C:7]2[O:16][C:11]3=[N:12][CH:13]=[CH:14][CH:15]=[C:10]3[C:9](=[O:17])[C:8]=2[CH:18]=1)#N.[C:19]([OH:22])(=[O:21])[CH3:20]>Cl>[O:17]=[C:9]1[C:10]2[C:11](=[N:12][CH:13]=[CH:14][CH:15]=2)[O:16][C:7]2[CH:6]=[CH:5][C:4]([CH2:20][C:19]([OH:22])=[O:21])=[CH:18][C:8]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 12274184HCID 12274184, 화합물

생성물 1

HCID 12274185HCID 12274185, 화합물

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of 12 g of 7-cyanomethyl-5-oxo-5H-[1]benzopyrano[2,3-b]-pyridine in a mixture of 60 ml of acetic acid and 25 ml of concentrated hydrochloric acid is heated under reflux on an oil bath for 24 hours. After concentration, water is added to the residue, and further a 10% sodium hydroxide solution is added to dissolve the residue. An insoluble material is removed by extraction with chloroform. The aqueous layer is made acid with acetic acid, and the resulting crystalline precipitate is filtered off and recrystallized from aqueous dimethylformamide to give 8.6 g of 5-oxo-5H-[1]benzopyrano[2,3-b]pyridin-7-yl-acetic acid as white needles melting at 244°- 245°C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux on an oil bath for 24 hours
  3. concentrationAfter concentration, water
  4. additionis added to the residue
  5. additionfurther a 10% sodium hydroxide solution is added
  6. dissolutionto dissolve the residue
  7. customAn insoluble material is removed by extraction with chloroform
  8. filtrationthe resulting crystalline precipitate is filtered off
  9. customrecrystallized from aqueous dimethylformamide

출처 및 근거

ORD 기록
ord-de5b21b15196437f859268de3411c8de
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931205

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