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Hydrochloric Acid → 1-[4-(6-Ethoxy-7,8-dimethyl-3-phenylimidazo[1,2-b]pyridazin-2-yl)phenyl]-cyclobutanamine

HRID 1501365
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HRID 1501365 반응식
[CH2:1]([O:3][C:4]1[C:5]([CH3:38])=[C:6]([CH3:37])[C:7]2[N:8]([C:10]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)=[C:11]([C:13]3[CH:18]=[CH:17][C:16]([C:19]4([NH:23]C(=O)OC(C)(C)C)[CH2:22][CH2:21][CH2:20]4)=[CH:15][CH:14]=3)[N:12]=2)[N:9]=1)[CH3:2].CO.Cl.O1CCOCC1>C(Cl)Cl>[CH2:1]([O:3][C:4]1[C:5]([CH3:38])=[C:6]([CH3:37])[C:7]2[N:8]([C:10]([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)=[C:11]([C:13]3[CH:14]=[CH:15][C:16]([C:19]4([NH2:23])[CH2:20][CH2:21][CH2:22]4)=[CH:17][CH:18]=3)[N:12]=2)[N:9]=1)[CH3:2]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 312751,4-DioxaneHCID 70856688HCID 70856688, 화합물

생성물 1

HCID 708178331-[4-(6-Ethoxy-7,8-dimethyl-3-phenylimidazo[1,2-b]pyridazin-2-yl)phenyl]-cyclobutanamine수율 82%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

To a mixture of the tert-butyl {1-[4-(6-ethoxy-7,8-dimethyl-3-phenylimidazo[1,2-b]pyridazin-2-yl)phenyl]cyclobutyl}carbamate that was prepared in a manner analgous to that described for Intermediate Example Int-36 (210 mg, 0.410 mmol, 1.0 eq) in DCM (2.64 mL) and MeOH (1.66 mL) was added a solution of 4 M hydrogen chloride in dioxane (2.05 mL, 8.19 mmol, 20.0 eq) and the mixture was stirred overnight at rt. The mixture was poured onto ice, made alkaline, treated with DCM and filtered through a phase separator. The volatile components of the organic phase were removed in vacuo to give 145 mg (82% yield) of the title compound.

후처리

  1. customwas prepared in a manner analgous to
  2. additionThe mixture was poured onto ice
  3. filtrationfiltered through a phase separator
  4. customThe volatile components of the organic phase were removed in vacuo

출처 및 근거

ORD 기록
ord-21df9bc34e2c49ed829ccbf7c8a82588
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206185B2

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