Toluene → HCID 57977987, 화합물

HRID 1865821노트

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HRID 1865821 반응식
C([N:8]1[C:13](=[O:14])[C:12]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)=[C:11]([C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=2)[C:10]([O:29]CC2C=CC=CC=2)=[N:9]1)C1C=CC=CC=1.C1(C)C=CC=CC=1.[Cl-].[Al+3].[Cl-].[Cl-]>O>[Cl:28][C:25]1[CH:24]=[CH:23][C:22]([C:11]2[C:10](=[O:29])[NH:9][NH:8][C:13](=[O:14])[C:12]=2[C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)=[CH:27][CH:26]=1

참가 물질

5

반응물 3

HCID 1140TolueneHCID 6451240Aluminum(III) ChlorideHCID 57977995HCID 57977995, 화합물

생성물 1

HCID 57977987HCID 57977987, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

To a round bottom flask was added 2-benzyl-6-(benzyloxy)-4,5-bis(4-chlorophenyl)pyridazin-3(2H)-one (15.5 gm, 30.21 mmol), toluene (70 ml) and aluminum chloride (10.08 gm, 75.54 mmol). The reaction was stirred at 90° C. for 2 h. After this time, the reaction was cooled to 0° C. and water (200 ml) was slowly added to the reaction. The solution was extracted with ethyl acetate (3 L). The organic layer was washed with water (200 ml) and saturated aqueous NaCl (200 ml). The organic layer was dried (MgSO4), filtered and concentrated. The title compound, 4,5-bis(4-chlorophenyl)-1,2-dihydropyridazine-3,6-dione, was obtained as a solid and used in next reaction without further purification. MS (M+H)=330.9, 333.0.

후처리

  1. temperatureAfter this time, the reaction was cooled to 0° C.
  2. extractionThe solution was extracted with ethyl acetate (3 L)
  3. washThe organic layer was washed with water (200 ml) and saturated aqueous NaCl (200 ml)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8853d20efa6743e5ada7f64b94c889a3
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629342B2

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