Potassium Carbonate → HCID 18447087、化合物

HRID 1269830ノート

反応式

HRID 1269830 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH:3]([O:7][C:8]2[CH:9]=[C:10]3[C:14](=[CH:15][CH:16]=2)[NH:13][N:12]=[CH:11]3)[CH2:2]1.I[CH2:18][CH2:19][OH:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[NH:13]1[C:14]2[C:10](=[CH:9][C:8]([O:7][CH:3]3[CH2:4][CH2:5][CH2:6][N:1]([CH2:18][CH2:19][OH:20])[CH2:2]3)=[CH:16][CH:15]=2)[CH:11]=[N:12]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12225IodoethanolHCID 229334705-[(Piperidin-3-yl)oxy]-1H-indazole

生成物 1

HCID 18447087HCID 18447087、化合物収率 32.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of the 5-(piperidin-3-yloxy)-1H-indazole (43 mg, 0.20 mmol) obtained in Example 377, 2-iodoethanol (84 mg, 0.49 mmol), potassium carbonate (70 mg, 0.50 mmol) and N,N-dimethylformamide (1 ml) was stirred at room temperature for 24 hours. The precipitate was removed by filtration and the solvent was distilled off as an azeotrope with toluene. The residue oil was purified by a silica gel column chromatography (eluent: ethyl acetate/triethylamine/ethanol=20/1/1) to obtain 2-[3-(1H-indazol-5-yloxy)piperidin-1-yl]ethanol (17 mg, 32%).

後処理

  1. customThe precipitate was removed by filtration
  2. distillationthe solvent was distilled off as an azeotrope with toluene
  3. customThe residue oil was purified by a silica gel column chromatography (eluent: ethyl acetate/triethylamine/ethanol=20/1/1)

出典と根拠

ORDレコード
ord-81101633bea04796bf77b730117a6211
出典データセット
uspto-grants-2007_04
特許番号
US07199147B2

反応ノート

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