Hydrochloric Acid → 2-(5-oxo-5H-chromeno[2,3-b]pyridin-7-yl)propanoic acid

HRID 1579447노트

반응식

HRID 1579447 반응식
[C:1]([C:3]([C:10]1[CH:11]=[CH:12][C:13]2[O:22][C:17]3=[N:18][CH:19]=[CH:20][CH:21]=[C:16]3[C:15](=[O:23])[C:14]=2[CH:24]=1)(C)[C:4]([O:6]CC)=[O:5])#N.Cl>C(O)(=O)C>[O:23]=[C:15]1[C:16]2[C:17](=[N:18][CH:19]=[CH:20][CH:21]=2)[O:22][C:13]2[CH:12]=[CH:11][C:10]([CH:3]([CH3:1])[C:4]([OH:6])=[O:5])=[CH:24][C:14]1=2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21568519Ethyl 2-cyano-2-(5-oxo-5H-[1]benzopyrano[2,3-b]pyridin-7-yl)propanoate

생성물 1

HCID 122741862-(5-oxo-5H-chromeno[2,3-b]pyridin-7-yl)propanoic acid수율 79.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 16.5 g of ethyl 2-cyano-2-(5-oxo-5H-[1]benzopyrano-[2,3-b]pyridin-7-yl)propionate, 80 ml of acetic acid and 35 ml of concentrated hydrochloric acid is heated under reflux 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 crystalline precipitate is collected and recrystallized from aqueous dioxane to give 11 g of 2-(5-oxo-5H-[1]benzopyrano[2,3-b]pyridin-7-yl)propionic acid as white needles melting at 194°-195°C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux 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. customthe crystalline precipitate is collected
  9. customrecrystallized from aqueous dioxane

출처 및 근거

ORD 기록
ord-af16e595e58d40709ffa73c54e7cb429
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931205

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