Piperazine → 1-(5-Isoquinolinylsulfonyl)piperazine

HRID 638371

반응식

HRID 638371 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[CH:13]1[C:22]2[CH:21]=[CH:20][CH:19]=[C:18]([S:23](Cl)(=[O:25])=[O:24])[C:17]=2[CH:16]=[CH:15][N:14]=1.C(Cl)(Cl)Cl>C(Cl)Cl>[CH:13]1[C:22]2[CH:21]=[CH:20][CH:19]=[C:18]([S:23]([N:1]3[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]3)(=[O:25])=[O:24])[C:17]=2[CH:16]=[CH:15][N:14]=1

참가 물질

6

반응물 4

HCID 4837PiperazineHCID 6212ChloroformHCID 11430Potassium CarbonateHCID 33716555-Isoquinolinesulfonyl chloride

생성물 1

HCID 35451-(5-Isoquinolinylsulfonyl)piperazine수율 89%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

In 100 ml of methylene chloride were added 6.0 g of piperazine and 1.2 g of anhydrous potassium carbonate, and to the mixture was added dropwise 30 ml of a methylene chloride solution containing 2.0 g of 5-isoquinolinesulfonyl chloride under cooling with ice. After the dropwise addition of the methylene chloride solution, the mixed solution was stirred at a temperature of 15° C. to 25° C. for 15 hours, and then the reaction solution was washed with water, dried with anhydrous magnesium sulfate, and the methylene chloride was distilled therefrom. The residue thus obtained was subjected to a silica gel column chromatography (silica gel: 70 g; solvent: chloroform) to give 2.14 g of 1-(5-isoquinolinesulfonyl)piperazine, i.e., Compound (35) in a yield of 89%.

후처리

  1. temperatureunder cooling with ice
  2. washthe reaction solution was washed with water
  3. dry with materialdried with anhydrous magnesium sulfate
  4. distillationthe methylene chloride was distilled
  5. customThe residue thus obtained

출처 및 근거

ORD 기록
ord-5cdcb99a0a934aacbffcd5dc00983cd9
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04560755

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