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

HRID 1579438
ノート
印刷プレビュー

反応式

HRID 1579438 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 176Acetic AcidHCID 12274195HCID 12274195、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-182892d7f348424fa54a2ff801de0448
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931205

反応ノート

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