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Acetic Acid → 2-(5H-chromeno[2,3-b]pyridin-7-yl)acetic acid

HRID 1579438
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반응식

HRID 1579438 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[CH2:9][C:8]=2[CH:17]=1)#N.[C:18]([OH:21])(=[O:20])[CH3:19]>Cl>[N:12]1[CH:13]=[CH:14][CH:15]=[C:10]2[CH2:9][C:8]3[CH:17]=[C:4]([CH2:19][C:18]([OH:21])=[O:20])[CH:5]=[CH:6][C:7]=3[O:16][C:11]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 12274195HCID 12274195, 화합물

생성물 1

HCID 3230052-(5H-chromeno[2,3-b]pyridin-7-yl)acetic acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of 11.5 g of 7-cyanomethyl-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 for 24 hours. After concentration, water is added to the residue, and further 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. The crystals are recrystallized from dioxane to give 8.5 g of 5H-[1]benzopyrano[2,3-b]-pyridin-7-yl-acetic acid as white needles melting at 218°C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 24 hours
  3. concentrationAfter concentration, water
  4. additionis added to the residue, and further 10% sodium hydroxide solution
  5. additionis 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. customThe crystals are recrystallized from dioxane

출처 및 근거

ORD 기록
ord-182892d7f348424fa54a2ff801de0448
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931205

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