Potassium Carbonate → HCID 59716641、化合物

HRID 2224224ノート

反応式

HRID 2224224 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 59716641HCID 59716641、化合物収率 99.8%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f1ecadf3c1ad477f927a6a8408a0f8bc
出典データセット
uspto-grants-2008_05
特許番号
US07378418B2

反応ノート

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