Potassium Carbonate → Ethyl (4-{[(6-chloro-3-{[(3-chlorophenyl)methyl]oxy}-2-fluorophenyl)carbonyl]amino}phenyl)acetate

HRID 1879122ノート

反応式

HRID 1879122 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5]Br.[Cl:10][C:11]1[C:16]([C:17]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:22][CH:21]=2)=[O:18])=[C:15]([F:32])[C:14]([OH:33])=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:10][C:11]1[C:16]([C:17]([NH:19][C:20]2[CH:21]=[CH:22][C:23]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:24][CH:25]=2)=[O:18])=[C:15]([F:32])[C:14]([O:33][CH2:5][C:4]2[CH:7]=[CH:8][CH:9]=[C:2]([Cl:1])[CH:3]=2)=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 698381-(Bromomethyl)-3-chlorobenzeneHCID 59163346Ethyl (4-{[(6-chloro-2-fluoro-3-hydroxyphenyl)carbonyl]amino}phenyl)acetate

生成物 1

HCID 59163349Ethyl (4-{[(6-chloro-3-{[(3-chlorophenyl)methyl]oxy}-2-fluorophenyl)carbonyl]amino}phenyl)acetate収率 84%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-Chlorobenzylbromide (28 μl, 0.24 mmol) was added to a suspension of ethyl (4-{[(6-chloro-2-fluoro-3-hydroxyphenyl)carbonyl]amino}phenyl)acetate (80 mg, 0.228 mmol) and potassium carbonate (38 mg, 0.273 mmol) in dimethylformamide (3 ml) and the reaction was stirred at room temperature for 4 hrs. The solvent was evaporated and the residue partitioned between water and ethyl acetate. The organic layer was separated, dried (Na2SO4) and the solvent evaporated to afford the title compound as a colourless oil (91 mg, 84%).

後処理

  1. customThe solvent was evaporated
  2. customthe residue partitioned between water and ethyl acetate
  3. customThe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. customthe solvent evaporated

出典と根拠

ORDレコード
ord-779175e7488842cea6f093149d9b45c7
出典データセット
uspto-grants-2012_11
特許番号
US08314147B2

反応ノート

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