1-(5-Isoquinolinylsulfonyl)piperazine → HCID 13116936、化合物

HRID 638375

反応式

HRID 638375 の反応式
[CH:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([S:11]([N:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)(=[O:13])=[O:12])[C:5]=2[CH:4]=[CH:3][N:2]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:26](Br)[CH3:27].CO.C(Cl)(Cl)Cl>C(O)C.C(Cl)(Cl)Cl>[CH:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([S:11]([N:14]3[CH2:19][CH2:18][N:17]([CH2:26][CH3:27])[CH2:16][CH2:15]3)(=[O:12])=[O:13])[C:5]=2[CH:4]=[CH:3][N:2]=1

参加物

7

反応物 4

HCID 35451-(5-Isoquinolinylsulfonyl)piperazineHCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 21584188Chloroform methanol

生成物 1

HCID 13116936HCID 13116936、化合物収率 74.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6212Chloroform溶媒

実験手順

In 100 ml of ethanol were added 2.77 g of 1-(5-isoquinolinesulfonyl)piperazine, i.e., Compound (35), 1.66 g of anhydrous potassium carbonate and 5.45 g of ethyl bromide, and the reaction was carried out at an external temperature of 70° C. for 24 hours. After the reaction solution was filtered, the filtrate was condensed and the residue was dissolved in 50 ml of chloroform, and the solution was extracted twice with a 2N aqueous hydrochloric acid solution. The aqueous hydrochloric acid layer was rendered alkaline, extracted twice with 50 ml of chloroform, and the chloroform layer extracted was washed with water and dried with anhydrous magnesium sulfate. After the chloroform was distilled therefrom, the residue obtained was subjected to a silica gel column chromatography (silica gel: 100 g; solvent: 2% methanol-chloroform) to give 2.26 g of 1-(5-isoquinolinesulfonyl)-4-ethylpiperazine, i.e., Compound (42) in a yield of 74%.

後処理

  1. filtrationAfter the reaction solution was filtered
  2. customcondensed
  3. extractionthe solution was extracted twice with a 2N aqueous hydrochloric acid solution
  4. extractionextracted twice with 50 ml of chloroform
  5. extractionthe chloroform layer extracted
  6. washwas washed with water
  7. dry with materialdried with anhydrous magnesium sulfate
  8. distillationAfter the chloroform was distilled
  9. customthe residue obtained

出典と根拠

ORDレコード
ord-118dcab10db243cba38965d8a598788b
出典データセット
uspto-grants-1985_12
特許番号
US04560755

関連ノート

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