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

HRID 2379582노트

반응식

HRID 2379582 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ab10a1e566a84a898678b668befeeae7
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05362738

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