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Hydrochloric Acid → 1-{4-[7,8-Dimethyl-6-(methylsulfanyl)-3-phenylimidazo[1,2-b]pyridazin-2-yl]-phenyl}cyclobutanamine

HRID 1501364
ノート
印刷プレビュー

反応式

HRID 1501364 の反応式
[CH3:1][C:2]1[C:7]([S:8][CH3:9])=[N:6][N:5]2[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]=[C:4]2[C:3]=1[CH3:37].CO.Cl.O1CCOCC1>C(Cl)Cl>[CH3:1][C:2]1[C:7]([S:8][CH3:9])=[N:6][N:5]2[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])[CH2:22][CH2:21][CH2:20]4)=[CH:17][CH:18]=3)[N:12]=[C:4]2[C:3]=1[CH3:37]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 312751,4-DioxaneHCID 70856623HCID 70856623、化合物

生成物 1

HCID 708179531-{4-[7,8-Dimethyl-6-(methylsulfanyl)-3-phenylimidazo[1,2-b]pyridazin-2-yl]-phenyl}cyclobutanamine収率 94%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

To a mixture of the tert-butyl (1-{4-[7,8-dimethyl-6-(methylsulfanyl)-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-35 (95 mg, 0.190 mmol, 1.0 eq) in DCM (1.19 mL) and MeOH (0.75 mL) was added a solution of 4 M hydrogen chloride in dioxane (0.92 mL, 3.69 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 75 mg (94% yield) of the title compound.

後処理

  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

出典と根拠

ORDレコード
ord-5aa3c7cfbc1644f7bd64904d81a2dd5d
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206185B2

反応ノート

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