2-Hydroxy-1,2,3-propanetricarboxylic acid hydrate (1:1) → HCID 178513084, compound

HRID 1449374Notes

Reaction equation

HRID 1449374 reaction equation
[C:1]1([C:10]([NH:12][C:13]([NH2:15])=[NH:14])=[O:11])[N:6]=[C:5]([Cl:7])[C:4]([NH2:8])=[N:3][C:2]=1[NH2:9].O.O.Cl.O.[C:20]([OH:32])(=[O:31])[CH2:21][C:22]([CH2:27][C:28]([OH:30])=[O:29])([C:24]([OH:26])=[O:25])[OH:23].C1(C(NC(N)=N)=O)N=C(Cl)C(N)=NC=1N>O>[C:1]1([C:10]([NH:12][C:13]([NH2:15])=[NH:14])=[O:11])[N:6]=[C:5]([Cl:7])[C:4]([NH2:8])=[N:3][C:2]=1[NH2:9].[C:20]([O-:32])(=[O:31])[CH2:21][C:22]([CH2:27][C:28]([O-:30])=[O:29])([C:24]([O-:26])=[O:25])[OH:23]

Participants

5

Reactant 3

HCID 222302-Hydroxy-1,2,3-propanetricarboxylic acid hydrate (1:1)HCID 178479506HCID 178479506, compoundHCID 178513083HCID 178513083, compound

Product 1

HCID 178513084HCID 178513084, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

Two millimoles of amiloride hydrochloride (604.0 mg) are dissolved in 150 ml of water, with gentle heating and filtered. One millimole of citric acid monohydrate (210.0 mg) is dissolved in 10 ml of water and added to the amiloride solution. The pH of this solution is pH 2.7. `The solution is stored at 5° C. for about 24 hours. The precipitate is washed with 2 ten milliter portions of water and then dried in vacuo at 40° C. After being further dried at 65° C. for 8 hours, the resulting amiloride citrate weighed 330 mg.

Workup

  1. temperaturewith gentle heating
  2. filtrationfiltered
  3. washThe precipitate is washed with 2 ten milliter portions of water
  4. customdried in vacuo at 40° C
  5. customAfter being further dried at 65° C. for 8 hours

Sources & evidence

ORD record
ord-5e35558fc67440cfa7ece560f6a693c5
Source dataset
uspto-grants-1980_02
Patent number
US04190655

Reaction notes

Loading…