6-Bromonaphthalene-2-sulfonyl chloride → 1-(6-Bromonaphthalene-2-sulfonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine

HRID 278593노트

반응식

HRID 278593 반응식
[CH:1]([N:4]([CH2:8][C:9]1[CH:22]=[CH:21][C:12]([C:13]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)=[O:14])=[CH:11][CH:10]=1)[CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[Br:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[CH:30]=[C:29]([S:34](Cl)(=[O:36])=[O:35])[CH:28]=[CH:27]2>C(=O)([O-])O.[Na+].C(OCC)(=O)C>[Br:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[CH:30]=[C:29]([S:34]([N:18]1[CH2:19][CH2:20][N:15]([C:13](=[O:14])[C:12]3[CH:21]=[CH:22][C:9]([CH2:8][N:4]([CH:5]([CH3:7])[CH3:6])[CH:1]([CH3:2])[CH3:3])=[CH:10][CH:11]=3)[CH2:16][CH2:17]1)(=[O:36])=[O:35])[CH:28]=[CH:27]2

참가 물질

5

반응물 2

HCID 144577416-Bromonaphthalene-2-sulfonyl chlorideHCID 226279521-(4-Diisopropylaminomethylbenzoyl)piperazine

생성물 1

HCID 226279921-(6-Bromonaphthalene-2-sulfonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine수율 59.9%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

To a mixture of 1-(4-diisopropylaminomethylbenzoyl)piperazine (200 mg) in 10% sodium hydrogen carbonate solution (10 ml) and ethyl acetate (15 ml), was added 6-bromonaphthalene-2-sulfonylchloride (179 mg), and the solution was stirred at room temperature for 30 minutes. The organic layer was separated, washed with water and extracted with 1 N hydrochloric acid. The extract was made alkaline with sodium hydroxide solution and extracted with dichloromethane. The extract was dried and concentrated. The residue was crystallized with ether to give the title compound (201 mg), as colorless crystals.

후처리

  1. customThe organic layer was separated
  2. washwashed with water
  3. extractionextracted with 1 N hydrochloric acid
  4. extractionextracted with dichloromethane
  5. customThe extract was dried
  6. concentrationconcentrated
  7. customThe residue was crystallized with ether

출처 및 근거

ORD 기록
ord-7207ae2e68a44ed68f7c777a00adbed8
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359134B1

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