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Hydrochloric Acid → 3-[3-Chloro-4-(6-methyl-pyridin-2-yl)-thiophen-2-yl]-8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazine, hydrochloride salt

HRID 1432665
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HRID 1432665 반응식
C1COCC1.Br[C:7]1[C:8]([Cl:28])=[C:9]([C:12]2[N:16]3[N:17]=[C:18]([CH3:26])[CH:19]=[C:20]([CH:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[C:15]3=[N:14][C:13]=2[CH3:27])[S:10][CH:11]=1.Br[C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([CH3:36])[N:31]=1.Cl.CCO>C(OCC)(=O)C.[Zn].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[ClH:28].[Cl:28][C:8]1[C:7]([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([CH3:36])[N:31]=2)=[CH:11][S:10][C:9]=1[C:12]1[N:16]2[N:17]=[C:18]([CH3:26])[CH:19]=[C:20]([CH:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[C:15]2=[N:14][C:13]=1[CH3:27]
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참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 8028TetrahydrofuranHCID 792052-Bromo-6-methylpyridineHCID 579330783-(4-Bromo-3-chloro-thiophen-2-yl)-8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazine

생성물 1

HCID 131727720
3-[3-Chloro-4-(6-methyl-pyridin-2-yl)-thiophen-2-yl]-8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazine, hydrochloride salt
수율 19.7%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매HCID 8857Ethyl Acetate용매

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온도
65 °C

실험 절차

Reike® Zn (0.5 g/mL solution in THF (1.9 mL, 1.45 mmol) is added to a flask containing 3-(4-bromo-3-chloro-thiophen-2-yl)-8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.30 g, 0.73 mmol). The slurry is heated at 65° C. for 1 hour, placed in a centrifuge for 5 minutes, and the resulting solution is transferred to a flask containing 2-bromo-6-methyl-pyridine (0.12 g, 0.73 mmol) and PdCl2(dppf) (0.018 g, 0.024 mmol). The reaction is heated at 65° C. overnight, diluted with ethyl acetate (20 mL), and washed with a sat. solution of NH4Cl (15 mL). The organic layer is dried over MgSO4, filtered, and concentrated. The residue is purified by silica gel chromatography using a hexanes and ethyl acetate gradient. The resulting product is dissolved in dichloromethane (5 mL), treated with a 1 M solution of HCl in EtOH (0.35 mL, 0.35 mmol) and concentrated. The residue is recrystallized from ethyl acetate and hexanes furnish the title compound (0.033 g, 0.072 mmol, 11%). 1H-NMR (CDCl3), δ 0.95 (t, J=7.3 Hz, 6H), 1.73-2.02 (m, 4H), 2.68 (s, 3H), 2.81 (s, 3H), 3.21 (s, 3H), 3.88-3.98 (m, 1H), 7.25 (s, 1H), 7.65 (d, J=7.5 Hz, 1H), 8.09 (d, J=7.5 Hz, 1H), 8.33 (dd, J=7.5, 7.1 Hz, 1H), 9.26 (s, 1H) ppm. LC/MS (m/z): calcd. for C23H26Cl2N4S (M+H)+: 424.2; found: 424.2.

후처리

  1. customthe resulting solution is transferred to a flask
  2. temperatureThe reaction is heated at 65° C. overnight
  3. washwashed with a sat. solution of NH4Cl (15 mL)
  4. dry with materialThe organic layer is dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is purified by silica gel chromatography
  8. dissolutionThe resulting product is dissolved in dichloromethane (5 mL)
  9. concentrationconcentrated
  10. customThe residue is recrystallized from ethyl acetate and hexanes

출처 및 근거

ORD 기록
ord-c6926cefbcf14f3fafd23a9510ea66e3
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612067B2

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