Potassium Carbonate → HCID 18447087, 화합물

HRID 1269830노트

반응식

HRID 1269830 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 18447087HCID 18447087, 화합물수율 32.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-81101633bea04796bf77b730117a6211
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199147B2

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