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Sodium Hydroxide → 2-[3-Chloro-6-[3-[4-(diphenylmethyl) piperazino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic acid

HRID 1169074
ノート
印刷プレビュー

反応式

HRID 1169074 の反応式
Cl.Cl.Cl.[Cl:4][C:5]1[N:9]2[N:10]=[C:11]([NH:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][N:21]([CH:24]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[CH2:20][CH2:19]3)[CH:12]=[CH:13][C:8]2=[N:7][C:6]=1[C:37]([CH3:44])([CH3:43])[C:38]([O:40]CC)=[O:39].[OH-].[Na+]>C(O)C>[Cl:4][C:5]1[N:9]2[N:10]=[C:11]([NH:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2:19][CH2:20][N:21]([CH:24]([C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=4)[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[CH2:22][CH2:23]3)[CH:12]=[CH:13][C:8]2=[N:7][C:6]=1[C:37]([CH3:44])([CH3:43])[C:38]([OH:40])=[O:39]
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 14798Sodium HydroxideHCID 22989265Ethyl 2-[3-chloro-6-[3-[4-(diphenylmethyl)piperazino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate trihydrochloride

生成物 1

HCID 229892372-[3-Chloro-6-[3-[4-(diphenylmethyl) piperazino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic acid収率 91.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

633 mg of ethyl 2-[3-chloro-6-[3-[4-(diphenylmethyl)-1-piperazinyl]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate trihydrochloride was dissolved in 6 ml of ethanol; 2.31 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 1.5 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate; the water layer was adjusted to pH 5 by the addition of 1 N hydrochloric acid. Methanol was added; the crystal precipitated was collected by filtration, washed with water-ethyl acetate and dried to yield 462 mg of the title compound.

後処理

  1. customrefluxing for 1.5 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. additionthe water layer was adjusted to pH 5 by the addition of 1 N hydrochloric acid
  7. additionMethanol was added
  8. customthe crystal precipitated
  9. filtrationwas collected by filtration
  10. washwashed with water-ethyl acetate
  11. customdried

出典と根拠

ORDレコード
ord-e0d480f6fc4a465d8fdaf4ce4e74b711
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06627630B1

反応ノート

読み込み中…

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