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

HRID 278602
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인쇄 미리보기

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HRID 278602 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-39bb1184006143ad9ac88865de0648b5
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06359134B1

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