6-(2-(3-Fluorophenyl)piperidin-1-yl)-3-nitroimidazo[1,2-b]pyridazine → 6-(2-(3-Fluorophenyl)piperidin-1-yl)imidazo[1,2-b]pyridazin-3-amine

HRID 588540노트

반응식

HRID 588540 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][N:9]2[C:14]2[CH:15]=[CH:16][C:17]3[N:18]([C:20]([N+:23]([O-])=O)=[CH:21][N:22]=3)[N:19]=2)[CH:5]=[CH:6][CH:7]=1>CCO>[F:1][C:2]1[CH:3]=[C:4]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][N:9]2[C:14]2[CH:15]=[CH:16][C:17]3[N:18]([C:20]([NH2:23])=[CH:21][N:22]=3)[N:19]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

3

반응물 1

HCID 673076686-(2-(3-Fluorophenyl)piperidin-1-yl)-3-nitroimidazo[1,2-b]pyridazine

생성물 1

HCID 673077316-(2-(3-Fluorophenyl)piperidin-1-yl)imidazo[1,2-b]pyridazin-3-amine

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

A mixture of 6-(2-(3-fluorophenyl)piperidin-1-yl)-3-nitroimidazo[1,2-b]pyridazine (50 mg, 0.146 mmol) and SnCl2 dihydrate (165 mg, 0.732 mmol) in 5 mL EtOH was first stirred at 70° C. for 30 minutes, then cooled to ambient temperature and concentrated. EtOAc and water (10 mL each) were added to the solid residue, followed by Na2CO3 aqueous solution (2 mL×2 N) to obtain a phase break. The organic layer was separated, and the aqueous layer was extracted with EtOAc (3×10 mL). The combined organic layers was dried with Na2SO4 and concentrated to provide the product for the next step.

후처리

  1. temperaturecooled to ambient temperature
  2. concentrationconcentrated
  3. additionEtOAc and water (10 mL each) were added to the solid residue
  4. customto obtain a phase break
  5. customThe organic layer was separated
  6. extractionthe aqueous layer was extracted with EtOAc (3×10 mL)
  7. dry with materialThe combined organic layers was dried with Na2SO4
  8. concentrationconcentrated
  9. customto provide the product for the next step

출처 및 근거

ORD 기록
ord-699557daa08f43c69c9b8d0ad8f30fc5
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227975B2

반응 노트

불러오는 중…