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Hydrochloric Acid → 1-(3-((1-Methyl-1H-indazol-5-yl)methyl)imidazo[1,2-b]pyridazin-6-yl)ethanone

HRID 1959665
ノート
印刷プレビュー

反応式

HRID 1959665 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[CH:8][C:9]2[N:10]([C:12]([CH2:15][C:16]3[CH:17]=[C:18]4[C:22](=[CH:23][CH:24]=3)[N:21]([CH3:25])[N:20]=[CH:19]4)=[CH:13][N:14]=2)[N:11]=1)=[CH2:5])C.Cl>CC(O)=O>[CH3:25][N:21]1[C:22]2[C:18](=[CH:17][C:16]([CH2:15][C:12]3[N:10]4[N:11]=[C:6]([C:4](=[O:3])[CH3:5])[CH:7]=[CH:8][C:9]4=[N:14][CH:13]=3)=[CH:24][CH:23]=2)[CH:19]=[N:20]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 581904976-(1-Ethoxy-vinyl)-3-(1-methyl-1H-indazol-5-ylmethyl)-imidazo[1,2-b]pyridazine

生成物 1

HCID 581905161-(3-((1-Methyl-1H-indazol-5-yl)methyl)imidazo[1,2-b]pyridazin-6-yl)ethanone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 6-(1-ethoxy-vinyl)-3-(1-methyl-1H-indazol-5-ylmethyl)-imidazo[1,2-b]pyridazine (50 mg, 0.15 mmol) and HCl (0.15 mL, 0.15 mmol) in AcOH (10 mL) was heated at 50° C. for 3 h. The solvent was removed under reduced pressure. The residue was diluted with water and pH of solution was adjusted to around 8 with saturated NaHCO3 solution, then was extracted with DCM three times. Organic layers were combined, dried over Na2SO4 and concentrated. The crude product was used in the next step without purification (45 mg, 75%, 76% purity). LCMS (method A): [MH]+=306, tR=5.03 min.

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionThe residue was diluted with water and pH of solution
  3. extractionwas extracted with DCM three times
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customThe crude product was used in the next step without purification (45 mg, 75%, 76% purity)

出典と根拠

ORDレコード
ord-6141486339584182b2eeb1fe5f299451
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08410264B2

反応ノート

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