Chloroform → 1-(5-Isoquinolinesulfonyl)-2,5-dimethylpiperazine

HRID 1263337

반응식

HRID 1263337 반응식
[CH3:1][CH:2]1[CH2:7][NH:6][CH:5]([CH3:8])[CH2:4][NH:3]1.C(N(CC)CC)C.[CH:16]1[C:25]2[CH:24]=[CH:23][CH:22]=[C:21]([S:26](Cl)(=[O:28])=[O:27])[C:20]=2[CH:19]=[CH:18][N:17]=1.C(Cl)(Cl)Cl>C(Cl)Cl>[CH:16]1[C:25]2[CH:24]=[CH:23][CH:22]=[C:21]([S:26]([N:3]3[CH2:4][CH:5]([CH3:8])[NH:6][CH2:7][CH:2]3[CH3:1])(=[O:28])=[O:27])[C:20]=2[CH:19]=[CH:18][N:17]=1

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 78162,5-DimethylpiperazineHCID 8471TriethylamineHCID 33716555-Isoquinolinesulfonyl chloride

생성물 1

HCID 132291781-(5-Isoquinolinesulfonyl)-2,5-dimethylpiperazine수율 59.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

In 30 ml of methylene chloride were dissolved 1.75 g of 2,5-dimethylpiperazine and 1.53 g of triethylamine, and to the solution was added dropwise 20 ml of a methylene chloride solution containing 1.73 g of 5-isoquinolinesulfonyl chloride under cooling with ice. After the dropwise addition of the methylene chloride solution, the mixed solution obtained was stirred at a temperature of 5° C. to 10° C. for three hours, and then the reaction mixture solution was washed with water and dried with anhydrous magnesium sulfate. After the methylene chloride was distilled therefrom, the residue obtained was subjected to an alumina column chromatography (alumina: 50 g; solvent: chloroform) to give 1.38 g of 1-(5-isoquinolinesulfonyl)-2,5-dimethylpiperazine, Compound (40) in a yield of 59%.

후처리

  1. temperatureunder cooling with ice
  2. customthe mixed solution obtained
  3. washthe reaction mixture solution was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. distillationAfter the methylene chloride was distilled
  6. customthe residue obtained

출처 및 근거

ORD 기록
ord-79e9a1bc8d18483fac905478d42f27ff
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04456757

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