Potassium Carbonate → HCID 59716641, 화합물

HRID 2224224노트

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HRID 2224224 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[N:12][N:11]3[C:14](=[O:17])[NH:15][N:16]=[C:10]3[C:9]=2[C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=2)=[CH:4][CH:3]=1.[C:25]([O:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[CH2:35]Cl)(=[O:27])[CH3:26].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O>[C:25]([O:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[CH2:35][N:15]1[C:14](=[O:17])[N:11]2[N:12]=[CH:13][C:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)=[C:9]([C:18]3[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=3)[C:10]2=[N:16]1)(=[O:27])[CH3:26]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 43471802-(Chloromethyl)phenyl acetateHCID 111641617,8-bis(4-chlorophenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

생성물 1

HCID 59716641HCID 59716641, 화합물수율 99.8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

To a solution of the 7,8-bis(4-chlorophenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one, (800 mg, 2.24 mmol), prepared as described in Example 1, in 30 mL of DMF was added 2-(chloromethyl)phenyl acetate (497 mg, 2.69 mmol), followed by K2CO3 (619 mg, 4.48 mmol). The reaction was heated at 60° C. for overnight. After this time, the reaction was allowed to cool to RT and then was diluted with 250 mL of EtOAc. The resultant solution was washed with saturated aqueous NaCl (100 mL×3). The organic layer was dried over MgSO4, filtered, evaporated under reduced pressure to provide the title compound, 2-((7,8-bis(4-chlorophenyl)-3-oxo-[1,2,4]triazolo[4,3-b]pyridazin-2(3H)-yl)methyl)phenyl acetate, (1.13 gm) as a yellow solid.

후처리

  1. temperatureto cool to RT
  2. washThe resultant solution was washed with saturated aqueous NaCl (100 mL×3)
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f1ecadf3c1ad477f927a6a8408a0f8bc
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07378418B2

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