Sodium Hydroxide → [6-[3-[4-(Diphenylmethoxy)piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylic acid

HRID 1169104ノート

反応式

HRID 1169104 の反応式
C([O:4][C:5]([C:7]1[N:15]=[C:14]2[N:9]([N:10]=[C:11]([O:16][CH2:17][CH2:18][CH2:19][N:20]3[CH2:25][CH2:24][CH:23]([O:26][CH:27]([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)[C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH2:22][CH2:21]3)[CH:12]=[CH:13]2)[N:8]=1)=[O:6])(C)C.[OH-].[Na+]>O1CCCC1>[C:34]1([CH:27]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[O:26][CH:23]2[CH2:24][CH2:25][N:20]([CH2:19][CH2:18][CH2:17][O:16][C:11]3[CH:12]=[CH:13][C:14]4[N:9]([N:8]=[C:7]([C:5]([OH:6])=[O:4])[N:15]=4)[N:10]=3)[CH2:21][CH2:22]2)[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 53847838Isopropyl [6-[3-[4-(diphenylmethoxy) piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylate

生成物 1

HCID 22989225[6-[3-[4-(Diphenylmethoxy)piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylic acid収率 78.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1.85 g of isopropyl[6-[3-[4-(diphenylmethoxy)piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylate was dissolved in 18 ml of tetrahydrofuran; 3.8 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 3.5 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate; 1 N hydrochloric acid was added to adjust pH 4.5. The mixture was crystallized by the addition of ethanol-acetone (1:2), collected by filtration, washed with water and ethyl acetate and dried to yield 1.33 g of the title compound.

後処理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated under reduced pressure
  3. additionThe residue was diluted with water
  4. washwashed with ethyl acetate
  5. addition1 N hydrochloric acid was added
  6. customThe mixture was crystallized by the addition of ethanol-acetone (1:2)
  7. filtrationcollected by filtration
  8. washwashed with water and ethyl acetate
  9. customdried

出典と根拠

ORDレコード
ord-8779ebb16c324e6d8acfd9f938daeef6
出典データセット
uspto-grants-2003_09
特許番号
US06627630B1

反応ノート

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