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

HRID 1603881노트

반응식

HRID 1603881 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-46708ea962d740968b8542aea6ba0d32
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990142

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