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1-(2-Methoxyphenyl)piperazine → 6-(3-(4-(2-methoxyphenyl)piperazin-1-yl)propoxy)-1H-indazole

HRID 1750159
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HRID 1750159 반응식
ClC1C(Cl)=CC=CC=1C1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][O:18][C:19]2[CH:27]=[C:26]3[C:22]([CH:23]=[N:24][NH:25]3)=[CH:21][CH:20]=2)[CH2:11][CH2:10]1.[Na+].[I-].[CH3:30][O:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[N:38]1CCNCC1.CCN(C(C)C)C(C)C>CC#N>[CH3:30][O:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[N:38]1[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][O:18][C:19]2[CH:27]=[C:26]3[C:22]([CH:23]=[N:24][NH:25]3)=[CH:21][CH:20]=2)[CH2:13][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 13461-(2-Methoxyphenyl)piperazineHCID 5238Sodium IodideHCID 81531DiisopropylethylamineHCID 666337746-(3-(4-(2,3-dichlorophenyl)piperidin-1-yl)propoxy)-1H-indazole

생성물 1

HCID 565973626-(3-(4-(2-methoxyphenyl)piperazin-1-yl)propoxy)-1H-indazole수율 60%

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

실험 절차

A mixture of intermediate 44 (42.2 mg, 0.17 mmol) and NaI (49.5 mg, 0.33 mmol) in CH3CN (3 mL) was heated to reflux for 30 min and then cooled to rt. To this mixture was added intermediate 65 (35.0 mg, 0.18 mmol), followed then by DIEA (0.063 mL, 0.36 mmol). The resulting mixture was heated to reflux and stirred for 4 h. Precipitated crystals were filtered off and the filtrate was evaporated under reduced pressure. The residue was extracted with EtOAc. The combined EtOAc layers were washed with brine, dried over anhydrous Na2SO4, concentrated in vacuo and purified by ISCO to give 6-(3-(4-(2-methoxyphenyl)piperazin-1-yl)propoxy)-1H-indazole (compound 50) (36.6 mg, 60%). HPLC: 99%, RT 3.907 min. MS (ESI) m/z 367.20 [M+H]+.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 30 min
  3. temperatureThe resulting mixture was heated
  4. temperatureto reflux
  5. customPrecipitated crystals
  6. filtrationwere filtered off
  7. customthe filtrate was evaporated under reduced pressure
  8. extractionThe residue was extracted with EtOAc
  9. washThe combined EtOAc layers were washed with brine
  10. dry with materialdried over anhydrous Na2SO4
  11. concentrationconcentrated in vacuo
  12. custompurified by ISCO

출처 및 근거

ORD 기록
ord-f5a039376e6f4efaab283a78da415533
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156822B2

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