p-Toluenesulfonic acid monohydrate → HCID 178427659, compound

HRID 980015Notes

Reaction equation

HRID 980015 reaction equation
[NH:1]([CH2:5][CH2:6][NH:7][S:8]([C:11]1[C:12]2[CH:13]=[CH:14][N:15]=[CH:16][C:17]=2[CH:18]=[CH:19][CH:20]=1)(=[O:10])=[O:9])[C:2]([NH2:4])=[NH:3].O.[C:22]1([CH3:32])[CH:27]=[CH:26][C:25]([S:28]([OH:31])(=[O:30])=[O:29])=[CH:24][CH:23]=1>CO>[NH:1]([CH2:5][CH2:6][NH:7][S:8]([C:11]1[C:12]2[CH:13]=[CH:14][N:15]=[CH:16][C:17]=2[CH:18]=[CH:19][CH:20]=1)(=[O:10])=[O:9])[C:2]([NH2:4])=[NH:3].[CH3:32][C:22]1[CH:27]=[CH:26][C:25]([S:28]([OH:31])(=[O:30])=[O:29])=[CH:24][CH:23]=1

Participants

4

Reactant 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 178513008HCID 178513008, compound

Product 1

HCID 178427659HCID 178427659, compoundYield 76.2%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

50 ml of methanol was suspended 20.5 g of N-(2-guanidinoethyl)-5-isoquinolinesulfonamide, and the mixture solution was dissolved completely with 30 ml of methanol solution containing 13.32 g of p-toluenesulfonic acid hydrate. The methanol was distilled therefrom under reduced pressure, the crystalline residue was recrystallized from water to give 24.8 g of N-(2-guanidinoethyl)-5-isoquinoline-sulfonamide-p-toluenesulfonate in a yield of 76.1%. The melting point of the compound was the range from 148° C. to 149° C.

Workup

  1. distillationThe methanol was distilled
  2. customunder reduced pressure, the crystalline residue was recrystallized from water

Sources & evidence

ORD record
ord-e215fcb7524f406faa822ef1de4c3e9c
Source dataset
uspto-grants-1987_01
Patent number
US04634770

Reaction notes

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