Hydrochloride methanol → HCID 178496799, compound

HRID 462913Notes

Reaction equation

HRID 462913 reaction equation
Cl.Cl.Cl.NCCCNCCCCNC(=O)C(NC(=O)CCCCCCCCNC(N)=N)O.Cl.CO.Cl.Cl.Cl.[NH2:39][CH2:40][CH2:41][CH2:42][NH:43][CH2:44][CH2:45][CH2:46][CH2:47][NH:48][C:49](=[O:68])[CH:50]([NH:53][C:54](=[O:67])[CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][NH:63][C:64]([NH2:66])=[NH:65])[O:51][CH3:52]>CO>[NH2:39][CH2:40][CH2:41][CH2:42][NH:43][CH2:44][CH2:45][CH2:46][CH2:47][NH:48][C:49](=[O:68])[CH:50]([NH:53][C:54](=[O:67])[CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][NH:63][C:64]([NH2:66])=[NH:65])[O:51][CH3:52]

Participants

5

Reactant 3

HCID 21893726Hydrochloride methanolHCID 178478606HCID 178478606, compoundHCID 178496800HCID 178496800, compound

Product 1

HCID 178496799HCID 178496799, compoundYield 65%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 160 mg (0.31 mmole) of N-[4-(3-aminopropyl)aminobutyl]-2-(9-guanidinononanamido)-2-hydroxyethanamide trihydrochloride in 3.2 ml of anhydrous methanol was added 0.32 ml of 2N hydrogen chloride-methanol. The mixture was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure and the resulting white powder was purified in a manner as that in Example 7, using CM-Sephadex® C-25 (Na-type) and Sephadex® LH-20 to yield 107 mg (65% yield) of a white powder of N-[4-(3-aminopropyl)aminobutyl]-2-(9-guanidinononanamido)-2-methoxyethanamide trihydrochloride.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe resulting white powder was purified in a manner as that in Example 7

Sources & evidence

ORD record
ord-dacca442631d47569e890ef4f1a09e0e
Source dataset
uspto-grants-1985_05
Patent number
US04518532

Reaction notes

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