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Hydrochloric Acid → 7-acetyl-2-amino-5-oxo-5H-chromeno[2,3-b]pyridine-3-carboxylic acid

HRID 986762
ノート
印刷プレビュー

反応式

HRID 986762 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:22][C:11]3=[N:12][C:13]([NH2:21])=[C:14]([C:16]([O:18]CC)=[O:17])[CH:15]=[C:10]3[C:9](=[O:23])[C:8]=2[CH:24]=1)(=[O:3])[CH3:2].[OH-].[Na+].Cl>C(O)C.O>[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:22][C:11]3=[N:12][C:13]([NH2:21])=[C:14]([C:16]([OH:18])=[O:17])[CH:15]=[C:10]3[C:9](=[O:23])[C:8]=2[CH:24]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 13728611HCID 13728611、化合物

生成物 1

HCID 137286127-acetyl-2-amino-5-oxo-5H-chromeno[2,3-b]pyridine-3-carboxylic acid収率 93.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

In ethanol (3 l) was suspended ethyl 7-acetyl-2-amino-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine-3-carboxylate (46 g). To the suspension were added water (460 ml) and 1N sodium hydroxide (462 ml). The mixture was stirred at room temperature for 1.5 hour, then at 50°-55° C. for 2 hours. The precipitating crystals were collected by filtration, and washed with ethanol. The crystals thus obtained were suspended in warm water (about 2 l). To the suspension was added concentrated hydrochloric acid (20 ml), and the mixture was stirred for 20 minutes. Insoluble matter was collected by filtration, washed with water, followed by recrystallization from dimethylformamide-water to give 7-acetyl-2-amino-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine-3-carboxylic acid as colorless crystals (39.3 g). Melting point: >300° C.

後処理

  1. waitat 50°-55° C. for 2 hours
  2. filtrationThe precipitating crystals were collected by filtration
  3. washwashed with ethanol
  4. customThe crystals thus obtained
  5. stirringthe mixture was stirred for 20 minutes
  6. filtrationInsoluble matter was collected by filtration
  7. washwashed with water
  8. customfollowed by recrystallization from dimethylformamide-water

出典と根拠

ORDレコード
ord-e315e9a42d544c98937e7404ad3dcafe
出典データセット
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04716167

反応ノート

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