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1,4-Dioxane → 1-(4-Amidino benzoyl)-4-(2-naphthalenesulfonyl)piperazine

HRID 278602
ノート
印刷プレビュー

反応式

HRID 278602 の反応式
Cl.[CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[S:12]([N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)(=[O:14])=[O:13].O1CCOCC1.Cl.[C:28]([C:31]1[CH:39]=[CH:38][C:34]([C:35](Cl)=[O:36])=[CH:33][CH:32]=1)(=[NH:30])[NH2:29]>C(=O)(O)[O-].[Na+]>[C:28]([C:31]1[CH:39]=[CH:38][C:34]([C:35]([N:18]2[CH2:19][CH2:20][N:15]([S:12]([C:3]3[CH:4]=[CH:5][C:6]4[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=4)[CH:2]=3)(=[O:14])=[O:13])[CH2:16][CH2:17]2)=[O:36])=[CH:33][CH:32]=1)(=[NH:29])[NH2:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 312751,4-DioxaneHCID 226280844-Amidinobenzoylchloride hydrochlorideHCID 227218151-(Naphthalene-2-sulfonyl)piperazine hydrochloride

生成物 1

HCID 183822251-(4-Amidino benzoyl)-4-(2-naphthalenesulfonyl)piperazine収率 52.8%

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

To a solution of 1-(2-naphthalenesulfonyl)piperazine hydrochloride (313 mg) in sodium bicarbonate solution (20 ml)-dioxane (20 ml) was added 4-amidinobenzoyl chloride hydrochloride (219 mg) and the solution was stirred at room temperature for 30 minutes. The reaction solution was concentrated, to which were added dichloromethane and water. The organic layer was separated and extracted with 1 N hydrochloric acid. The extract was made alkaline with sodium hydroxide solution and the precipitate was filtered, washed with water and dried to give a colorless solid of the title compound (223 mg).

後処理

  1. concentrationThe reaction solution was concentrated, to which
  2. additionwere added dichloromethane and water
  3. customThe organic layer was separated
  4. extractionextracted with 1 N hydrochloric acid
  5. filtrationthe precipitate was filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-39bb1184006143ad9ac88865de0648b5
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06359134B1

反応ノート

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