Ammonia → 8-Nitro-4-oxo-4H-1-benzopyran-2-carboxamide

HRID 1603881ノート

反応式

HRID 1603881 の反応式
[NH3:1].[N+:2]([C:5]1[C:14]2[O:13][C:12]([C:15](OCC)=[O:16])=[CH:11][C:10](=[O:20])[C:9]=2[CH:8]=[CH:7][CH:6]=1)([O-:4])=[O:3]>C(O)C.O1CCCC1>[N+:2]([C:5]1[C:14]2[O:13][C:12]([C:15]([NH2:1])=[O:16])=[CH:11][C:10](=[O:20])[C:9]=2[CH:8]=[CH:7][CH:6]=1)([O-:4])=[O:3]

参加物

5

反応物 2

HCID 222AmmoniaHCID 100840998-nitro-2-ethoxycarbonyl-4-oxo-4H-1-benzopyran

生成物 1

HCID 196062688-Nitro-4-oxo-4H-1-benzopyran-2-carboxamide収率 81%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Gas ammonia was bubbled for 30 minutes in a solution of ethyl 8-nitro-4-oxo-4H-benzopyran-2-carboxylate (2.109 g, 8.02 mmol) in anhydrous ethanol (50 ml) and anhydrous tetrahydrofuran (50 ml). After that the mixture was evaporated to dryness and the resulting solid residue was suspended in concentrated hydrochloric acid (20 ml) stirring at room temperature for 4 h. Then the mixture was diluted with water, the solid was recovered by filtration, washed repeatedly with water and dried under vacuum on phosphorous pentoxyde, to obtain 1.515 g of the title product (81% yield).

後処理

  1. customAfter that the mixture was evaporated to dryness
  2. additionThen the mixture was diluted with water
  3. filtrationthe solid was recovered by filtration
  4. washwashed repeatedly with water
  5. customdried under vacuum on phosphorous pentoxyde

出典と根拠

ORDレコード
ord-46708ea962d740968b8542aea6ba0d32
出典データセット
uspto-grants-1999_11
特許番号
US05990142

反応ノート

読み込み中…