Sodium Hydroxide → 2-(6-((3-(4-(Diphenylmethoxy)piperidino)propyl)amino)imidazo(1,2-b)pyridazin-2-yl)-2-methylpropionic acid

HRID 1067510ノート

反応式

HRID 1067510 の反応式
[C:1]1([CH:7]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[O:8][CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19]3[CH:20]=[CH:21][C:22]4[N:23]([CH:25]=[C:26]([C:28]([CH3:35])([CH3:34])[C:29]([O:31]CC)=[O:30])[N:27]=4)[N:24]=3)[CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>C(O)C>[C:36]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[O:8][CH:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19]3[CH:20]=[CH:21][C:22]4[N:23]([CH:25]=[C:26]([C:28]([CH3:35])([CH3:34])[C:29]([OH:31])=[O:30])[N:27]=4)[N:24]=3)[CH2:13][CH2:14]2)[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 9872422Ethyl 2-[6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate

生成物 1

HCID 98069212-(6-((3-(4-(Diphenylmethoxy)piperidino)propyl)amino)imidazo(1,2-b)pyridazin-2-yl)-2-methylpropionic acid収率 60.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

468 mg of ethyl 2-[6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate was dissolved in 3 ml of ethanol; 2 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 15 hours. After 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 7 by the addition of 1 N hydrochloric acid, followed by extraction with ethyl acetate-tetrahydrofuran (1:1); the extract was washed with saturated saline and dried with magnesium sulfate. After the dry product was concentrated under reduced pressure, ethyl acetate was added to the residue; the crystal precipitated was collected by filtration, washed with ethyl acetate and dried to yield 267 mg of the title compound.

後処理

  1. concentrationAfter the mixture was concentrated under reduced pressure
  2. additionthe residue was diluted with water
  3. washwashed with ethyl acetate
  4. additionthe water layer was adjusted to pH 7 by the addition of 1 N hydrochloric acid
  5. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:1)
  6. washthe extract was washed with saturated saline
  7. dry with materialdried with magnesium sulfate
  8. concentrationAfter the dry product was concentrated under reduced pressure, ethyl acetate
  9. additionwas added to the residue
  10. customthe crystal precipitated
  11. filtrationwas collected by filtration
  12. washwashed with ethyl acetate
  13. customdried

出典と根拠

ORDレコード
ord-30f62615d27f4acd922b07e87c5ad81b
出典データセット
uspto-grants-2001_06
特許番号
US06248740B1

反応ノート

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