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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
ノート
印刷プレビュー

反応式

HRID 1432665 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 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

生成物 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
収率 19.7%

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c6926cefbcf14f3fafd23a9510ea66e3
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07612067B2

反応ノート

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