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 588540ノート

反応式

HRID 588540 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-699557daa08f43c69c9b8d0ad8f30fc5
出典データセット
uspto-grants-2016_01
特許番号
US09227975B2

反応ノート

読み込み中…