Sodium Hydroxide → 2-[6-[3-[4-(Diphenylmethylamino)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic Acid

HRID 1169091ノート

反応式

HRID 1169091 の反応式
[C:1]1([CH:7]([NH:14][CH:15]2[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][CH2:23][NH:24][C:25]3[CH:26]=[CH:27][C:28]4[N:29]([CH:31]=[C:32]([C:34]([CH3:41])([CH3:40])[C:35]([O:37]CC)=[O:36])[N:33]=4)[N:30]=3)[CH2:17][CH2:16]2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>C(O)C>[C:1]1([CH:7]([NH:14][CH:15]2[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][CH2:23][NH:24][C:25]3[CH:26]=[CH:27][C:28]4[N:29]([CH:31]=[C:32]([C:34]([CH3:41])([CH3:40])[C:35]([OH:37])=[O:36])[N:33]=4)[N:30]=3)[CH2:17][CH2:16]2)[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22989234Ethyl 2-[6-[3-[4-(diphenylmethylamino) piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate

生成物 1

HCID 229893972-[6-[3-[4-(Diphenylmethylamino)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic Acid収率 86.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

612 mg of ethyl 2-[6-[3-[4-(diphenylmethylamino)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate was dissolved in 5 ml of ethanol; 2.2 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 6 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was diluted with water, washed with ethyl acetate and adjusted to pH 5 by the addition of 1 N hydrochloric acid. The mixture was saturated with sodium chloride and extracted with tetrahydrofuran; the extract was dried over magnesium sulfate and concentrated under reduced pressure, powdered by the addition of ethyl ether, collected by filtration and dried to yield 503 mg of the title compound.

後処理

  1. customrefluxing for 6 hours
  2. temperatureAfter cooling
  3. concentrationthe mixture was concentrated under reduced pressure
  4. additionThe residue was diluted with water
  5. washwashed with ethyl acetate
  6. additionadjusted to pH 5 by the addition of 1 N hydrochloric acid
  7. extractionextracted with tetrahydrofuran
  8. dry with materialthe extract was dried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. additionpowdered by the addition of ethyl ether
  11. filtrationcollected by filtration
  12. customdried

出典と根拠

ORDレコード
ord-cc2139f450d64c7eb580edd828f4eb50
出典データセット
uspto-grants-2003_09
特許番号
US06627630B1

反応ノート

読み込み中…