Hydrochloric Acid → HCID 178479477, compound

HRID 980016Notes

Reaction equation

HRID 980016 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].[ClH:21].[OH-].[Na+]>O>[ClH:21].[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]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178513008HCID 178513008, compound

Product 1

HCID 178479477HCID 178479477, compoundYield 82%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

In 55 ml of water was suspended 20.5 g of N-(2-guanidinoethyl)-5-isoquinolinesulfonamide, the crystalline residue was dissolved by slowly adding of 8.2 ml of an aqueous concentrated hydrochloric acid solution. The pH of the aqueous layer was adjusted to 6.8 with 3.2 ml of a 10N aqueous sodium hydroxide solution by dropwise addition at a temperature of 30° C. to 40° C., and the mixed solution was stirred for a night. The crystalline residue thus obtained was separated by filtration, and the residue was recrystallized from 50 ml of water to give 18.9 g of N-(2-guanidinoethyl)-5-isoquinolinesulfonamide monohydrochloride in a yield of 82%. The melting point of the compound was 236° C.

Workup

  1. dissolutionthe crystalline residue was dissolved
  2. customThe crystalline residue thus obtained
  3. customwas separated by filtration
  4. customthe residue was recrystallized from 50 ml of water

Sources & evidence

ORD record
ord-e7eeba8e2090480d8dd95e7c5dfc11a5
Source dataset
uspto-grants-1987_01
Patent number
US04634770

Reaction notes

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