Water → HCID 178513008, 화합물

HRID 247584

반응식

HRID 247584 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 178513008HCID 178513008, 화합물수율 84.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-a3d115384dbb41d79a84fc75fcc3c33c
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709032

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