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Hydrochloric Acid → (Rac)-2-{4-[3-(1-quinolin-6-yl-ethyl)-imidazo[1,2-b]pyridazin-6-yl]-pyrazol-1-yl}-ethanol

HRID 69218
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인쇄 미리보기

반응식

HRID 69218 반응식
O1CCCCC1[O:7][CH2:8][CH2:9][N:10]1[CH:14]=[C:13]([C:15]2[CH:16]=[CH:17][C:18]3[N:19]([C:21]([CH:24]([C:26]4[CH:27]=[C:28]5[C:33](=[CH:34][CH:35]=4)[N:32]=[CH:31][CH:30]=[CH:29]5)[CH3:25])=[CH:22][N:23]=3)[N:20]=2)[CH:12]=[N:11]1.C(Cl)Cl.Cl.C([O-])(O)=O.[Na+]>O1CCOCC1.O.CC#N>[N:32]1[C:33]2[C:28](=[CH:27][C:26]([CH:24]([C:21]3[N:19]4[N:20]=[C:15]([C:13]5[CH:12]=[N:11][N:10]([CH2:9][CH2:8][OH:7])[CH:14]=5)[CH:16]=[CH:17][C:18]4=[N:23][CH:22]=3)[CH3:25])=[CH:35][CH:34]=2)[CH:29]=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 68641062(Rac)-6-[1-(6-{1-[2-(tetrahydro-pyran-2-yloxy)-ethyl]-1h-pyrazol-4-yl}-imidazo[1,2-b]pyridazin-3-yl)-ethyl]-quinoline

생성물 1

HCID 57917405(Rac)-2-{4-[3-(1-quinolin-6-yl-ethyl)-imidazo[1,2-b]pyridazin-6-yl]-pyrazol-1-yl}-ethanol

시약·촉매·용매 2

HCID 312751,4-Dioxane용매
HCID 18373917Acetonitrile--water (1/1)용매

실험 절차

In a flask were introduced (rac)-6-[1-(6-{1-[2-(tetrahydro-pyran-2-yloxy)-ethyl]-1H-pyrazol-4-yl}-imidazo[1,2-b]pyridazin-3-yl)-ethyl]-quinoline (Stage 177.1, 147 mg, 0.33 mmol) and DCM (4 mL), before adding dropwise HCl in dioxane (4 N, 0.248 mL). The RM was stirred at rt for 1 h and was then blown off with nitrogen. The residue was dissolved in water/CH3CN 1:1. The solution was basified with NaHCO3 (ca. 0.5 g) before being concentrated. The white suspension was filtered and the cake was washed with water, before being dried under vacuum. The crude was dissolved in MeOH/water and purified by preparative HPLC (H2O/CH3CN/TFA 1000:0:1 to 750:250:1 in 20 min.). Collected fractions containing the product were put together and basified with NaHCO3, before being concentrated. The resulting white suspension was filtered and the cake was washed with water, before being dried under high vacuum to give the title compound as a white solid (tR 1.83 min (conditions 8), MH+=360).

후처리

  1. concentrationbefore being concentrated
  2. filtrationThe white suspension was filtered
  3. washthe cake was washed with water
  4. custombefore being dried under vacuum
  5. dissolutionThe crude was dissolved in MeOH/water
  6. custompurified by preparative HPLC (H2O/CH3CN/TFA 1000:0:1 to 750:250:1 in 20 min.)
  7. additionCollected fractions containing the product
  8. concentrationbefore being concentrated
  9. filtrationThe resulting white suspension was filtered
  10. washthe cake was washed with water
  11. custombefore being dried under high vacuum

출처 및 근거

ORD 기록
ord-76b3502bdd7841f48fa2c9df3669a44b
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822468B2

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