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Sodium Bicarbonate → 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

HRID 2186175
ノート
印刷プレビュー

反応式

HRID 2186175 の反応式
Cl.Cl.[N:3]1([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH:25]4[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]4)[C:20](=[O:31])[CH2:19]3)(=[O:17])=[O:16])=[CH:11][CH:10]=2)[CH:7]=[CH:6][N:5]=[CH:4]1.Cl.Cl[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][N:35]=1.C(=O)(O)[O-].[Na+]>>[N:3]1([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH:25]4[CH2:30][CH2:29][N:28]([C:38]5[CH:37]=[CH:36][N:35]=[CH:34][CH:39]=5)[CH2:27][CH2:26]4)[C:20](=[O:31])[CH2:19]3)(=[O:16])=[O:17])=[CH:13][CH:14]=2)[CH:7]=[CH:6][N:5]=[CH:4]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 516892Sodium BicarbonateHCID 156199202-Chloropyridine--hydrogen chloride (1/1)HCID 234474334-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone Dihydrochloride

生成物 1

HCID 234475814-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone収率 48.4%

反応条件

温度
130 °C

実験手順

A mixture of 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone dihydrochloride (209 mg) and chloropyridine hydrochloride (93 mg) was added to sodium bicarbonate solution, and the mixture was extracted with dichloromethane (twice), dried and concentrated. To the residue was added isoamylalcohol (10 ml), and the mixture was stirred at 130° C. for 15 hours. The reaction solution was concentrated, and the residue was dissolved in dichloromethane. The solution was washed with 1N sodium hydroxide solution, dried and concentrated, and the residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution=7:1) to give colorless solid of 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone (102 mg). The obtained 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone was dissolved in ethyl acetate (5 ml), and to the solution was added a solution of 4N hydrochloric acid in ethyl acetate. Precipitates were filtered, washed with ethyl acetate and dried to give colorless solid of the title compound (103 mg).

後処理

  1. extractionthe mixture was extracted with dichloromethane (twice),
  2. customdried
  3. concentrationconcentrated
  4. additionTo the residue was added isoamylalcohol (10 ml)
  5. concentrationThe reaction solution was concentrated
  6. dissolutionthe residue was dissolved in dichloromethane
  7. washThe solution was washed with 1N sodium hydroxide solution
  8. customdried
  9. concentrationconcentrated
  10. customthe residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution=7:1)

出典と根拠

ORDレコード
ord-26b711e162304365b2940ad54fd9e62c
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06403595B1

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート