Piperazine → 1-(5-Isoquinolinylsulfonyl)piperazine

HRID 638371

反応式

HRID 638371 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 35451-(5-Isoquinolinylsulfonyl)piperazine収率 89%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-5cdcb99a0a934aacbffcd5dc00983cd9
出典データセット
uspto-grants-1985_12
特許番号
US04560755

関連ノート

読み込み中…