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

HRID 456156
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HRID 456156 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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 10 mL AcOH was heated at 50° C. for 3 hour. The solvent was removed under reduced pressure. The residue was diluted with water and adjusted the pH value of solution to around 8 with aqueous NaHCO3, 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% pure). LCMS (method A): [MH]+=306, tR=5.03 min.

후처리

  1. customThe solvent was removed under reduced pressure
  2. additionThe residue was diluted with water
  3. extractionextracted 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% pure)

출처 및 근거

ORD 기록
ord-7488dba1efe74934b7996af0cb5329f8
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08497368B2

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