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

HRID 1248759

反応式

HRID 1248759 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 132291781-(5-Isoquinolinesulfonyl)-2,5-dimethylpiperazine収率 59.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-020d59c94ab748d79eb7930b6789cd81
出典データセット
uspto-grants-1985_06
特許番号
US04525589

関連ノート

読み込み中…