Potassium Hydroxide → 9-chloro-6-imino-4-oxo-3-phenyl-6H-pyrido[2,1-a]isoindole-1-carboxylic acid

HRID 2379582ノート

反応式

HRID 2379582 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[N:7][N:8]3[C:15](=[O:16])[C:14]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=4)=[CH:13][C:12]([C:23]([OH:25])=[O:24])=[C:9]32)=[CH:4][CH:3]=1.[OH-].[K+]>CO>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[NH:7])[N:8]3[C:15](=[O:16])[C:14]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=4)=[CH:13][C:12]([C:23]([OH:25])=[O:24])=[C:9]32)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 1895709410-chloro-4-oxo-3-phenyl-4H-pyrido[2,1-a]phthalazine-1-carboxylic acid

生成物 1

HCID 189570979-chloro-6-imino-4-oxo-3-phenyl-6H-pyrido[2,1-a]isoindole-1-carboxylic acid収率 94.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.5 g of 10-chloro-4-oxo-3-phenyl-4H-pyrido[2,1-a]-phthalazine-1-carboxylic acid were added to a solution of 5.6 g of potassium hydroxide in 60 ml of methanol, whereupon the mixture was heated to boiling under reflux for 25 hours. The solvent was then removed in a vacuum and the residue was taken up in 60 ml of water. The product was precipitated by the addition of 2N hydrochloric acid. The crystals were filtered off under suction, washed with water and dried in a vacuum. There was obtained 3.32 g of 9-chloro-6-imino-4-oxo-3-phenyl-6H-pyrido[2,1-a]isoindole-1-carboxylic acid as yellowish crystals with a m.p. of 266°-268° (decomposition).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 25 hours
  3. customThe solvent was then removed in a vacuum
  4. customThe product was precipitated by the addition of 2N hydrochloric acid
  5. filtrationThe crystals were filtered off under suction
  6. washwashed with water
  7. customdried in a vacuum

出典と根拠

ORDレコード
ord-ab10a1e566a84a898678b668befeeae7
出典データセット
uspto-grants-1994_11
特許番号
US05362738

反応ノート

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