Potassium Carbonate → 2-[(Pyridin-2-yl)methyl]-7-[4-[3-[9-(2,2,2-trifluoroethylcarbamoyl)-9H-fluoren-9-yl]propyl]piperazin-1-yl]-3,4-dihydro-2H-isoquinolin-1-one

HRID 1796766ノート

反応式

HRID 1796766 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][N:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][C:12]([N:18]3[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]3)=[CH:13][CH:14]=2)[C:9]1=[O:31].C(=O)([O-])[O-].[K+].[K+].[F:38][C:39]([F:62])([F:61])[CH2:40][NH:41][C:42]([C:44]1([CH2:57][CH2:58][CH2:59]Br)[C:56]2[CH:55]=[CH:54][CH:53]=[CH:52][C:51]=2[C:50]2[C:45]1=[CH:46][CH:47]=[CH:48][CH:49]=2)=[O:43]>CN(C=O)C.C(OCC)(=O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][N:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][C:12]([N:18]3[CH2:19][CH2:20][N:21]([CH2:59][CH2:58][CH2:57][C:44]4([C:42](=[O:43])[NH:41][CH2:40][C:39]([F:38])([F:61])[F:62])[C:56]5[CH:55]=[CH:54][CH:53]=[CH:52][C:51]=5[C:50]5[C:45]4=[CH:46][CH:47]=[CH:48][CH:49]=5)[CH2:22][CH2:23]3)=[CH:13][CH:14]=2)[C:9]1=[O:31]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 105977593-[9-(2,2,2-Trifluoroethylcarbamoyl)-9H-fluoren-9-yl]propyl bromideHCID 221804472-[(pyridin-2-yl)methyl]-7-(4-tert-butoxycarbonyl-piperazin-1-yl)-3,4-dihydro-2H-isoquinolin-1-one

生成物 1

HCID 221801892-[(Pyridin-2-yl)methyl]-7-[4-[3-[9-(2,2,2-trifluoroethylcarbamoyl)-9H-fluoren-9-yl]propyl]piperazin-1-yl]-3,4-dihydro-2H-isoquinolin-1-one収率 71%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
8 °C

実験手順

The compound (50 mg, 0.16 mmol) prepared in step (b) of Example 125 was dissolved in anhydrous DMF. Potassium carbonate (44 mg) and 66 mg of the compound prepared in step (a) of Example 93 were added to the solution. The mixture was stirred at 50° C. for 20 hr and further at 8° C. for 4.5 hr. The reaction solution was diluted with ethyl acetate, and the dilution was washed twice with water, followed by drying over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography (development system, methylene chloride:methanol=30:1) to give the title compound (46 mg, yield 71%) as a white foam.

後処理

  1. washthe dilution was washed twice with water
  2. dry with materialby drying over anhydrous magnesium sulfate
  3. customThe solvent was removed by distillation under the reduced pressure
  4. customThe residue was purified by column chromatography (development system, methylene chloride:methanol=30:1)

出典と根拠

ORDレコード
ord-284c9d0a1b5447b0a2f312ad9b2557f0
出典データセット
uspto-grants-2006_04
特許番号
US07030120B2

反応ノート

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