Water → HCID 178513008、化合物

HRID 247584

反応式

HRID 247584 の反応式
[NH2:1][CH2:2][CH2:3][NH:4][S:5]([C:8]1[C:9]2[CH:10]=[CH:11][N:12]=[CH:13][C:14]=2[CH:15]=[CH:16][CH:17]=1)(=[O:7])=[O:6].O.S(O)(O)(=O)=O.CS[C:26](=[NH:28])[NH2:27].[OH-].[Na+]>CO>[NH:1]([CH2:2][CH2:3][NH:4][S:5]([C:8]1[C:9]2[CH:10]=[CH:11][N:12]=[CH:13][C:14]=2[CH:15]=[CH:16][CH:17]=1)(=[O:7])=[O:6])[C:26]([NH2:28])=[NH:27]

参加物

6

反応物 4

HCID 962WaterHCID 3544N-(2-Aminoethyl)isoquinoline-5-sulfonamideHCID 14798Sodium HydroxideHCID 752702-Methyl-2-thiopseudourea sulfate

生成物 1

HCID 178513008HCID 178513008、化合物収率 84.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 30 ml of methanol was dissolved 3.3 g of N-(2-aminoethyl)-5-isoquinolinesulfonamide obtained in Referential example 1, and to the solution was added 25 ml of water solution containing 5.0 g of S-methylisothiourea sulfate. And to the mixed solution was added 1N aqueous sodium hydroxide solution, the mixed solution thus obtained was heated at reflux for two hours. After the reflux, the methanol was distilled therefrom under reduced pressure, and the white crystals precipitated were separated by filtration under reduced pressure. The crystalline residue thus obtained was recrystallized from methanol to give 3.24 g of N-(2-guanidinoethyl)-5-isoquinolinesulfonamide, i.e., Compound (2) in a yield of 84%.

後処理

  1. customobtained in Referential example 1
  2. customthe mixed solution thus obtained
  3. temperaturewas heated
  4. temperatureat reflux for two hours
  5. distillationAfter the reflux, the methanol was distilled
  6. customunder reduced pressure, and the white crystals precipitated
  7. customwere separated by filtration under reduced pressure
  8. customThe crystalline residue thus obtained
  9. customwas recrystallized from methanol

出典と根拠

ORDレコード
ord-a3d115384dbb41d79a84fc75fcc3c33c
出典データセット
uspto-grants-1987_11
特許番号
US04709032

関連ノート

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