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Sodium Bicarbonate → 4-[5-(4-Chlorophenyl)-2-thiophenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

HRID 2186164
ノート
印刷プレビュー

反応式

HRID 2186164 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]([S:14]([N:17]3[CH2:22][CH2:21][N:20]([CH2:23][CH:24]4[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]4)[C:19](=[O:30])[CH2:18]3)(=[O:16])=[O:15])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.Cl.Cl[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=1.C(=O)(O)[O-].[Na+]>>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]([S:14]([N:17]3[CH2:22][CH2:21][N:20]([CH2:23][CH:24]4[CH2:29][CH2:28][N:27]([C:37]5[CH:36]=[CH:35][N:34]=[CH:33][CH:38]=5)[CH2:26][CH2:25]4)[C:19](=[O:30])[CH2:18]3)(=[O:16])=[O:15])=[CH:11][CH:10]=2)=[CH: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 234473094-[5-(4-Chlorophenyl)-2-thiophenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride

生成物 1

HCID 234474724-[5-(4-Chlorophenyl)-2-thiophenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

反応条件

温度
130 °C

実験手順

To 1-[1-(tert-butoxycarbonyl)piperidin-4-ylmethyl]-4-[5-(4-chlorophenyl)-2-thiophenesulfonyl]-2-piperazinone (115 mg) were added 4N hydrochloric acid in ethyl acetate (10 ml) and methanol (4 ml), and the mixture was stirred at room temperature for 30 minutes. The reaction solution was concentrated to give crude crystals of 4-[5-(4-chlorophenyl)-2-thiophenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride. A mixture of the obtained 4-[5-(4-chlorophenyl)-2-thiophenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride and chloropyridine hydrochloride (85 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=10:1) to give colorless solid of the title compound (42 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=10:1)

出典と根拠

ORDレコード
ord-b71c4b1bff904759862c43a98430d54c
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

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